반응 #329200

반응 방정식

water

(±)-methyl 2-(prop-2-en-1-yloxy)propanoate

trimethylaluminum

N-methyl-O-methyl hydroxylamine hydrochloride

→

titled compound

(±)-N-methoxy-N-methyl-2-(prop-2-en-1-yloxy)propanamide

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도The mixture was warmed to ambient temperature
2. 2
   workup.STIRRINGstirred for an additional 14 hours
3. 3
   추출extracted with dichloromethane (2×300 mL)
4. 4
   건조The combined organic extracts were dried with sodium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated in vacuo

실험 절차

A suspension of N-methyl-O-methyl hydroxylamine hydrochloride (10.0 g, 104 mmol, 2 equiv) in dichloromethane (100 mL) was treated with trimethylaluminum (52.0 mL, 104 mmol, 2 equiv) at 0° C. After stirring for 1 hour at 0° C., a dichloromethane (50 mL) solution of (±)-methyl 2-(prop-2-en-1-yloxy)propanoate (7.50 g, 52.0 mmol) was added over 15 minutes. The mixture was warmed to ambient temperature and stirred for an additional 14 hours. The mixture was treated with water (500 mL) and extracted with dichloromethane (2×300 mL). The combined organic extracts were dried with sodium sulfate, filtered, and concentrated in vacuo to provide the titled compound.

출처