Tag: 33100-27-5

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.33100-27-5,1,4,7,10,13-Pentaoxacyclopentadecane,as a common compound, the synthetic route is as follows.

EXAMPLE 1 A mixture of 1-[3-(naphth-2-ylmethoxy)phenyl]cyclohexanol (0.65 g), sodium hydride (0.096 g of a 50percent w/w dispersion in mineral oil), 1,4,7,10,13-pentaoxacyclopentadecane (hereinafter 15-crown-5, (0.06 g) and tetrahydrofuran (10 ml) was stirred at ambient temperature for 15 minutes. methyl iodide (0.12 ml) was added and the mixture was stirred at ambient temperature for 15 hours. The mixture was evaporated and the residue was partitioned between diethyl ether and water. The organic layer was separated, washed with a saturated aqueous sodium chloride solution, dried (MgSO4 and evaporated. The residue was purified by column chromatography using a 9:1 v/v mixture of methylene chloride and diethyl ether as eluent. There was thus obtained 1-methoxy-1-[3-(naphth-2-ylmethoxy)phenyl]cyclohexane (0.35 g, 54percent), m.p. 74-75¡ãC. The 1-[3-(naphth-2-ylmethoxy)phenyl]cyclohexanol starting material was obtained as follows:-.

The synthetic route of 33100-27-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; IMPERIAL CHEMICAL INDUSTRIES PLC; ICI-PHARMA; EP375452; (1994); B1;,
Chiral Catalysts
Chiral catalysts – SlideShare

33100-27-5, 1,4,7,10,13-Pentaoxacyclopentadecane is a chiral-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A suspension of H3MST (323mg, 0.467mmol) and NaH (34.7mg, 1.45mmol) in 5mL of DMA was allowed to stir for 45min. After H2 evolution ceased, In(OAc)3 (137mg, 0.469mmol) was added and the solution stirred vigorously. After 2h, 5mL of Et2O was added and the solution stirred for an additional 30min, followed by filtration (see Note). The filtrate was concentrated to dryness under reduced pressure, then the residue was triturated with Et2O and dried to afford a white precipitate. The solid was collected in a medium-porosity glass fritted funnel, washed with Et2O and pentane, and dried in vacuo to yield 356mg (?90percent) of a white powder, which was used without further purification. 1H NMR (500MHz, DMSO-d6, ppm): 2.22 (s, 9H), 2.52 (br t, 6H), 2.58 (s, 18H), 2.80 (br t, 6H), 6.87 (s, 6H). A suspension of this white powder that was assumed to be [InMST] (117mg, 0.145mmol), NaOH (6.3mg, 0.16mmol) and 15-crown-5 (46muL, 0.23mmol) in 4mL THF was allowed to stir for 8h, after which the mixture was filtered with a medium-porosity glass fritted funnel into a vial. Diethyl ether was slowly allowed to diffuse into the vial and within 1day a white powdery residue formed, which was removed via filtration and the filtrate was again exposed to Et2O vapor. Over the next 5days colorless crystals formed, which were collected, washed with Et2O, and dried in vacuo to yield 65mg (40percent) of the product. 1H NMR (500MHz, CDCl3, ppm): 1.79 (s, OH), 2.26 (s, 9H), 2.58 (t, 6H), 2.72 (s, 18H), 2.92 (t, 6H), 3.62 (m, 20H), 6.87 (s, 6H). 13C{1H} NMR (500MHz, CDCl3, ppm): 21.0, 23.6, 40.2, 52.9, 69.4, 131.4, 136.5, 139.4, 140.0. FTIR (Nujol, selected bands, cm?1) nu(OH) 3561; 1602, 1563, 1113, 975, 817, 653. Anal. Calc. for [15-crown-5?NaI-(mu-OH)-InIIIMST], C47H76InN4NaO13S3: C, 49.24; H, 6.64; N, 5.10. Found: C, 49.56; H, 6.72; N, 4.92percent.

The synthetic route of 33100-27-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Sickerman, Nathaniel S.; Henry, Rene?e M.; Ziller, Joseph W.; Borovik; Polyhedron; vol. 58; (2013); p. 65 – 70;,
Chiral Catalysts
Chiral catalysts – SlideShare

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.33100-27-5,1,4,7,10,13-Pentaoxacyclopentadecane,as a common compound, the synthetic route is as follows.

Sodium hydride (60percent dispersion in mineral oil, 0.14 g) was added portionwise to a stirred solution of a portion (0.87 g) of the 3-hydroxypyrrolidine so obtained and 1,4,7,10,13-pentaoxacyclopentadecane (hereinafter 15-crown-5, 0.05 g) in DMF (10 ml). The mixture was stirred at ambient temperature for 15 minutes. A solution of methyl 4-toluenesulphonate (0-56 g) in THF (2 ml) was added dropwise and the mixture was stirred at ambient temperature for 2 hours. The mixture was partitioned between diethyl ether and water. The organic phase was dried (Na2 SO4) and evaporated. The residue was purified by column chromatography using increasingly polar mixtures of hexane and ethyl acetate as eluent. There was thus obtained 1-benzyl-3-(3,5-difluorophenyl)-3-methoxypyrrolidine (0.82 g, 90percent).

33100-27-5 1,4,7,10,13-Pentaoxacyclopentadecane 36336, achiral-catalyst compound, is more and more widely used in various.

Reference£º
Patent; Zeneca Limited; Zeneca Pharma S.A.; US5420298; (1995); A;,
Chiral Catalysts
Chiral catalysts – SlideShare

33100-27-5, 1,4,7,10,13-Pentaoxacyclopentadecane is a chiral-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 8 Synthesis of 4-(4-fluorobenzylidene)piperidine hydrochloride To a stirred suspension of 13.20 g of 60percent sodium hydride (in oil) containing 1.65 g of 15-crown-5 ether in 650 ml of tetrahydrofuran were added dropwise a solution of 59.78 g of N-t-butoxycarbonylpiperidone and 81.25 g of diethyl 4-fluorobenzylphosphonate in 150 ml of tetrahydrofuran under ice-cooling over 20 minutes. After stirring at room temperature for a day, a saturated aqueous sodium bicarbonate solution was added cautiously, followed by extracting with ethyl acetate. The extract was washed with a saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution, successively, and dried over anhydrous sodium sulfate, followed by removal of the drying agent by filtration. The filtrate was concentrated under reduced pressure and purified by a flash column chromatography (silica gel: Wakogel C200 (manufactured by Wako Pure Chemicals), eluent; hexane-ethyl acetate =20:1) to give 55.23 g of N-t-butoxycarbonyl-4-(4-fluorobenzylidene)piperidine as an oil, which was then crystallized by allowing to stand at room temperature overnight. m.p. 69-70¡ãC. To 55.00 g of N-t-butoxycarbonyl-4-(4-fluorobenzylidene)piperidine was added 475 ml of an ice-cooled solution of 4 N hydrogen chloride in dioxane, followed by stirring at room temperature for 2 hours. The reaction solution was concentrated under reduced pressure, and the resulting crystals were recrystallized from isopropanol to give 40.72 g of 4-(4-fluorobenzylidene)piperidine hydrochloride. m.p. 184-185.5¡ã C.

33100-27-5 1,4,7,10,13-Pentaoxacyclopentadecane 36336, achiral-catalyst compound, is more and more widely used in various.

Reference£º
Patent; Taisho Pharmaceutical Co., Ltd.; Nihon Nohyaku Co. Ltd.; US6291467; (2001); B1;,
Chiral Catalysts
Chiral catalysts – SlideShare

33100-27-5, 1,4,7,10,13-Pentaoxacyclopentadecane is a chiral-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A solution of (2 mmol, 0.4 ml) of 15-crown-5 in (10 ml) of absolute ethanol was added to a solution of (1 mmol, 0.933 gm Pr-picrate), (0.936 gm Nd-picrate) and (0.900 gm Dy-picrate) in (10 ml) of absolute ethanol and refluxed at (50 ? 60 oC) for (1 hr.). The solution was concentrated at (40 ? 50 oC) to a very small volume (till the formation of a precipitate), usually a gummy precipitate forms which was treated with (40 ? 60 oC) petroleum ether until all the gummy precipitate was converted to a fine yellow ? orange powder. The precipitate was collected and stored in a desicator for complete dryness. These complexes were also prepared by another method, by stirring a solution of 15-crown-5 with a solution of lanthanide picrate for (24 ? 48 hrs.). The gummy precipitates were treated with petroleum ether. The yields were (92 ? 96percent)24.

33100-27-5 1,4,7,10,13-Pentaoxacyclopentadecane 36336, achiral-catalyst compound, is more and more widely used in various.

Reference£º
Article; Al-Amery, Mohammed H. A.; Al-Abdaly, B. Ibrahim; Albayaty, M. Kahtan; Oriental Journal of Chemistry; vol. 32; 2; (2016); p. 1025 – 1048;,
Chiral Catalysts
Chiral catalysts – SlideShare

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.33100-27-5,1,4,7,10,13-Pentaoxacyclopentadecane,as a common compound, the synthetic route is as follows.

General procedure: Crystals of compounds 1?3 were prepared by isothermal evaporation fromaqueous solutions at room temperature. The crystals of compound 1 weresynthesized by the reaction of 0.051 g (0.1 mmol) of UO2(NO3)2¡¤6H2O,0.040 g (0.22 mmol) of 12-crown-4, 0.280 g (2.0 mmol) of 40percent H2SeO4,and 2.001 g (111.2 mmol) of deionized distilled water. Compound 2:0.050 g (0.1 mmol) of uranyl nitrate, 0.046 g (0.21 mmol) of 15-crown-5,0.282 g (2.0 mmol) of selenic acid, and 2.012 g (111.7 mmol) of deionizeddistilled water. Compound 3: 0.050 g (0.1 mmol) of uranyl nitrate, 0.046 g(0.21 mmol) of 15-crown-5, 0.282 g (2.0 mmol) of selenic acid, and 2.012 g(111.7 mmol) of deionized distilled water (note: the bulk of crystals herebelongs to compound 2). Homogeneous liquid solutions were left in awatch glass. Yellowish-green flattened crystals formed within 2 weeks.

The synthetic route of 33100-27-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Gurzhiy, Vladislav V.; Tyumentseva, Olga S.; Tyshchenko, Darya V.; Krivovichev, Sergey V.; Tananaev, Ivan G.; Mendeleev Communications; vol. 26; 4; (2016); p. 309 – 311;,
Chiral Catalysts
Chiral catalysts – SlideShare

33100-27-5, 1,4,7,10,13-Pentaoxacyclopentadecane is a chiral-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 3 Production of 1-(2,6-dichloro-4-trifluoromethylphenyl)-4-methylsulfenyl-5-(1-oxy-pyridin-3-ylmethylamino)pyrazole-3-carbonitrile (Compound No. 14) In 10 ml of N,N-dimethylformamide was suspended 0.1 g of 60percent sodium hydride, and 1 g of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfinylpyrazole-3-carbonitrile was gradually added thereto. After 20 minutes of stirring at room temperature, 3 drops of 15-crown-5-ether and then 0.3 g of 3-chloromethylpyridine-1-oxide were added thereto, followed by stirring at room temperature. After standing over one night, water and ethyl acetate were added thereto and the mixture was neutralized by 1N hydrochloric acid. After liquid separation, the organic layer was washed with saturated saline and then dried over anhydrous sodium sulfate. The residue was purified by a silica gel column chromatography to obtain 0.9 g of the compound (No. 14) described in the following Table 1.

33100-27-5 1,4,7,10,13-Pentaoxacyclopentadecane 36336, achiral-catalyst compound, is more and more widely used in various.

Reference£º
Patent; MITSUBISHI CHEMICAL CORPORATION; US2003/60471; (2003); A1;,
Chiral Catalysts
Chiral catalysts – SlideShare