Реакция #84031

Уравнение реакции

potassium carbonate

CO2

N,O-Dimethylhydroxylamine Hydrochloride

6-bromo-2-naphthoyl chloride

→

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

Выход 100.0%

Растворители

dichloromethane

Water

water

dichloromethane

Условия реакции

Обработка

1. 1
   workup.STIRRINGThe reaction mixture was stirred 1 hour
2. 2
   ДругоеThe organic layer was separated
3. 3
   Сушкаdried over sodium sulphate
4. 4
   Фильтрацияfiltrated
5. 5
   Концентрированиеconcentrated
6. 6
   Другоеdried in vacuum overnight

Методика

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.

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