S-(2,4-DIMETHYLPHENYL) ETHANETHIOATE synthesis

Yield:94602-20-7 100%

Reaction Conditions:

with pyridine in dichloromethane at 5 - 15; for 1 h;

Steps:

1 Preparation of S-(2,4-dimethylphenyl) ethanethioate

100 g of 2,4 dimethyl thiophenol was suspended in 500 ml of dichloromethane and added 94 gm of pyridine at 25°C. Reaction mixture was cooled to 5-10°C and then drop wise added acetyl chloride (64 gm, 0.815 mole). Resulting reaction mixture was heated at 5 - 15°C for 1 hr. RM was monitored by HPLC. When reaction was completed cooled to RT, added waterand stined for 10 - 20 mins. Desired product was extracted with ethyl acetate twice. Combined organic layer was washed with water, brine, dried over sodium sulfate and concentrated under reduced pressure to give oily mass as desired product (130 gm, 100%).

References:

WO2016/135636,2016,A1 Location in patent:Page/Page column 18; 19