Hydrochloric Acid → 4,4,4-Trifluorobutyl thioacetate

温度

80 °C

A mixture of 23.80 g of 1-iodo-4,4,4-trifluorobutane, 100 ml of N,N-dimethylformamide and 11.42 g of potassium thioacetate was heated and stirred at 80° C. for 4 hours under a nitrogen atmosphere. A reaction vessel was cooled in an ice bath. To the reaction mixture was added an aqueous 1N hydrochloric acid solution, and the mixture was extracted with 100 ml of t-butyl methyl ether twice. Organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over sodium sulfate, filtered, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 18.20 g of 4,4,4-trifluorobutyl thioacetate represented by the formula:

1. temperaturewas heated
2. temperatureA reaction vessel was cooled in an ice bath
3. extractionthe mixture was extracted with 100 ml of t-butyl methyl ether twice
4. washwashed with an aqueous saturated sodium chloride solution
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure

ORDレコード

ord-0e41ff9cecd64e4b89e4f03e0560501c

出典データセット

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08247596B2