Acetic acid, 2-chloro-2,2-difluoro-, ethyl ester → Ethyl 2,2-difluoro-2-(methylsulfanyl)acetate

A solution of ethyl chlorodifluoroacetate (7.9 g, 50.0 mmol) in dimethyl sulfoxide (20 ml) was added dropwise to a solution of sodium methyl mercaptan (4.6 g, 65 mmol) in dimethyl sulfoxide (60 ml) under cooling with ice, and the mixture was stirred at room temperature for 1 hour. After completion of the reaction, the reaction mixture was poured into ice water to conduct extraction with ether. The solvent was distilled out of the resultant extract under reduced pressure. The resultant residue was distilled under reduced pressure to obtain the intended product (3.7 g; yield: 43.2%) as a colorless oil.

1. temperatureunder cooling with ice
2. customAfter completion of the reaction
3. extractionextraction with ether
4. distillationThe solvent was distilled out of the resultant
5. extractionextract under reduced pressure
6. distillationThe resultant residue was distilled under reduced pressure
7. customto obtain the intended product (3.7 g; yield: 43.2%) as a colorless oil

ORD record

ord-64305ff4848b493a8ce35d10632e68f0

Source dataset

uspto-grants-2001_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06229049B1