Methanesulfonic acid, 1,1,1-trifluoro-, 4-phenyl-1-cyclohexen-1-yl ester synthesis

8synthesis methods

Product Name:Methanesulfonic acid, 1,1,1-trifluoro-, 4-phenyl-1-cyclohexen-1-yl ester
CAS Number:122948-47-4
Molecular formula:C13H13F3O3S
Molecular Weight:306.3

358-23-6 Synthesis

358-23-6
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4894-75-1
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Methanesulfonic acid, 1,1,1-trifluoro-, 4-phenyl-1-cyclohexen-1-yl ester

122948-47-4
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Yield:122948-47-4 89%

Reaction Conditions:

with 2,6-di-tert-butyl-4-methylpyridine in dichloromethane at 40; for 1 h;

Steps:

4

0.579 ml of trifluoromethanesulphonic anhydride (1.2 equivalents) is added dropwise to a solution of 0.5 g of 4-phenylcyclohexanone and 0.648 g of 2,6-di(tert-butyl)-4-methylpyridine (1.1 equivalents) in 8.0 ml of anhydrous dichloromethane. The reaction medium is subsequently stirred for 1 hour at 40° C., diluted with 25 ml of dichloromethane, washed with water (2×15 ml), dried over sodium sulphate, filtered and then concentrated under reduced pressure. Chromatography of the residue on silica gel (cyclohexane/ethyl acetate: 80/20) makes it possible to isolate 0.788 g of the expected product. Yield: 89% 1H NMR (CDCl3) δ (ppm): 1.92 (m, 1H), 2.05 (m, 1H), 2.35 (m, 4H), 2.80 (m, 1H), 5.80 (m, 1H), 7.15 (m, 3H), 7.22 (m, 2H)

References:

US2004/72871,2004,A1 Location in patent:Page/Page column 16

37595-74-7 Synthesis