Dimethylformamide → (3R)-2-(4-chloro-2-fluorophenyl)-4,4,4-trifluoro-3-methylbutanoyl chloride

660 mg (2.32 mmol) of (3R)-2-(4-chloro-2-fluorophenyl)-4,4,4-trifluoro-3-methylbutanoic acid (diastereomer mixture) were dissolved in 2 ml of dichloromethane. After addition of a small drop of DMF, the reaction solution was cooled to from −5° C. to 0° C., and 0.4 ml (4.64 mmol) of oxalyl chloride was added dropwise. Cooling was removed and the reaction mixture was stirred at RT for 1 h until the evolution of gas had ceased. The mixture was then concentrated under reduced pressure. The residue was twice taken up in abs. dichloromethane, in each case reconcentrated under reduced pressure and the residue was finally dried under high vacuum. This gave 640 mg of the target product which was directly, without further purification, reacted further.

1. additionwas added dropwise
2. temperatureCooling
3. customwas removed
4. concentrationThe mixture was then concentrated under reduced pressure
5. customthe residue was finally dried under high vacuum
6. customThis gave 640 mg of the target product which was directly, without further purification
7. customreacted further

ORDレコード

ord-f3d7d1415a83473c9bfc9385d388573c

出典データセット

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09018414B2