反応 #48876

反応方程式

dimethylamine

THF

2-chloro-4,5-difluorobenzoic acid

(1-chloro-2-methylprop-1-en-1-yl)dimethylamine

triethylamine

→

title compound

収率 96.8%

2-Chloro-4,5-difluoro-N,N-dimethylbenzamide

収率 96.8%

溶媒

DCM

DCM

hydrochloric acid

反応条件

後処理

1. 1
   その他separated
2. 2
   乾燥The organic layer was dried (MgSO4)
3. 3
   ろ過filtered
4. 4
   濃縮concentrated in vacuo

実験手順

A solution of 2-chloro-4,5-difluorobenzoic acid (385 mg, 2.0 mmol) in DCM (5 mL) was treated with (1-chloro-2-methylprop-1-en-1-yl)dimethylamine (293 mg, 2.2 mmol) and stirred under argon for 1 hour. The mixture was then treated with triethylamine (0.56 mL, 4.0 mmol) and a 2M solution of dimethylamine in THF (1.2 mL, 2.4 mmol), and stirred for 18 hours. The mixture was diluted with DCM (5 mL) and 2M hydrochloric acid (4 mL) and separated. The organic layer was dried (MgSO4), filtered and concentrated in vacuo to afford the title compound (425 mg). The residue was used without further purification.

出典