반응 #84031

반응 방정식

potassium carbonate

CO2

N,O-Dimethylhydroxylamine Hydrochloride

6-bromo-2-naphthoyl chloride

→

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

수율 100.0%

용매

dichloromethane

Water

water

dichloromethane

반응 조건

후처리

1. 1
   workup.STIRRINGThe reaction mixture was stirred 1 hour
2. 2
   기타The organic layer was separated
3. 3
   건조dried over sodium sulphate
4. 4
   여과filtrated
5. 5
   농축concentrated
6. 6
   기타dried in vacuum overnight

실험 절차

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.

출처