Extracurricular laboratory: Synthetic route of 29683-23-6

The synthetic route of 29683-23-6 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 29683-23-6, Tetrahydro-2H-thiopyran-4-ol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, category: alcohols-buliding-blocks, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks

Example 288: 4-[[(4-Chlorophenyl)sulfonyl](2,5-difluorophenyl)methyl]tetrahydrothiopyran The 2-[(4-chlorophenyl)sulfonylmethyl]-1,4-difluorobenzene (500 mg, 1.65 mmol) obtained in Example 5 and tetrahydrothiopyran-4-ol (400 mg, 3.38 mmol) were dissolved in toluene (20 ml), followed by the addition of cyanomethylenetri-n-butylphosphorane (800 mg, 3.31 mmol).. Under an argon atmosphere, the resulting mixture was heated under reflux for 14 hours.. After the reaction mixture was allowed to cool down, cyanomethylenetri-n-butylphosphorane (400 mg, 1.66 mmol) was added.. Under an argon atmosphere, the resulting mixture was heated under reflux for 14 hours.. The reaction mixture was then allowed to cool down.. The residue obtained by concentrating the reaction mixture under reduced pressure was subjected to flash silica gel chromatography, and the fraction obtained from the hexane:ethyl acetate=15:1 elude was concentrated under reduced pressure to give a white solid.. The white solid was washed with a hexane/diisopropyl ether mixture, whereby the title compound (404 mg, 1.00 mmol, 61%) was obtained as a white powder.1H-NMR (400 MHz, CDCl3) delta: 1.47(1H,ddd,J=23.4,10.0,3.3Hz), 1.68(1H,ddd,J=25.0,11.4,3.3Hz), 2.13(1H,dm,J=11.4Hz), 2.50-2.78(5H,m), 2.82(1H,td,J=12.8,2.6Hz), 4.47(1H,d,J=7.3Hz), 6.72-6.82(1H,m), 6.90-7.40(1H,m), 7.31(2H,d,J=8.8Hz), 7.40-7.60(1H,m), 7.49(2H,d,J=8.8Hz). IR (ATR) cm-1: 2939, 2887, 1576, 1493, 1425, 1317, 1281, 1240, 1142, 1084, 1012, 866, 831, 781, 750, 731, 710, 631, 615, 548, 467. mp: 150-152C. MS m/z: 403 (M++H).Anal. Calcd for C18H17ClF2O2S2: C, 53.66; H, 4.25; Cl, 8.80; F, 9.43; S, 15.92. Found: C, 53.52; H, 4.21; Cl, 9.00; F, 9.54; S, 15.88.

The synthetic route of 29683-23-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1466898; (2004); A1;,
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