Vinylidene chloride → 1,1,1-Trifluoro-4,4-dichloro-3-buten-2-one

温度

-50 °C

To a solution of aluminum chloride (3.0 g, 22.5 mmol) in dichloromethane (100 mL) was added dropwise a solution of trifluoroacetyl chloride (3 g, 22.6 mmol) in dichloro-methane (5 mL) while keeping the temperature of the reaction mixture below −30° C. The reaction mixture was stirred for 15 minutes at −50° C. Then a solution of vinylidene chloride (2.2 g, 22.7 mmol) in dichloromethane (10 mL) was added dropwise over 2 h to the reaction mixture. The reaction mixture was stirred an additional 2 h at −50° C. and then warmed gradually to room temperature. The reaction mixture was diluted with water, and the aqueous layer was extracted with dichloromethane. The organic layers were combined, dried (MgSO4), and concentrated under reduced pressure to give 4,4-dichloro-1,1,1-trifluoro-3-buten-2-one as an oil which was used for the next step without further purification.

1. customthe temperature of the reaction mixture below −30° C
2. stirringThe reaction mixture was stirred an additional 2 h at −50° C.
3. temperaturewarmed gradually to room temperature
4. extractionthe aqueous layer was extracted with dichloromethane
5. dry with materialdried (MgSO4)
6. concentrationconcentrated under reduced pressure

ORDレコード

ord-45a42197a6224ad4bf0c13449cad8107

出典データセット

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08449898B2