反応 #84031

反応方程式

potassium carbonate

CO2

N,O-Dimethylhydroxylamine Hydrochloride

6-bromo-2-naphthoyl chloride

→

6-bromo-N-methoxy-N-methyl-2-naphthamide

収率 100.0%

溶媒

dichloromethane

Water

water

dichloromethane

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction mixture was stirred 1 hour
2. 2
   その他The organic layer was separated
3. 3
   乾燥dried over sodium sulphate
4. 4
   ろ過filtrated
5. 5
   濃縮concentrated
6. 6
   その他dried in vacuum overnight

実験手順

N,O-Dimethylhydroxylamine Hydrochloride (41.3 g, 423 mmol, 1.5 equiv.) was dissolved in distilled water (200 mL) and potassium carbonate (117 g, 3.0 equiv.) was added portion wise (CO2 evolution). Water (300 mL) and dichloromethane (200 mL) was added and a solution of 6-bromo-2-naphthoyl chloride (76.1 g, 282 mmol, 1.00-equiv.) in dichloromethane (300 mL) was added portion wise to this mixture while stirring. The reaction mixture was stirred 1 hour. The organic layer was separated, dried over sodium sulphate, filtrated, concentrated and dried in vacuum overnight, yielding 6-bromo-N-methoxy-N-methyl-2-naphthamide (82.9 g, 100%) as a brown solid.

出典