تفاعل #985298

معادلة التفاعل

N,O-dimethyl-hydroxylamine HCl

Triethylamine

cyclopropanecarbonyl chloride

→

colorless oil

المردود 61.4%

Cyclopropanecarboxylic acid methoxy-methyl-amide

المردود 61.4%

المذيبات

DCM

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled in ice
2. 2
   درجة الحرارةwithout cooling
3. 3
   استخلاصExtraction
4. 4
   workup.DISTILLATIONDistillation
5. 5
   أخرى75° C./20 mbar

الإجراء التجريبي

N,O-dimethyl-hydroxylamine HCl (40 g, 410 mmol) was suspended under nitrogen in DCM (400 mL) and cooled in ice. Triethylamine (63 mL, 451 mmol) was added slowly, then cyclopropanecarbonyl chloride (41 mL, 451 mmol) was added slowly. Stirring without cooling was continued for 1 h. Extraction: 2×DCM, 1×1 N HCl, 1×NaCl. Distillation: 75° C./20 mbar. One obtained 32.5 g (61%) of a colorless oil.

المصدر