반응 #1166472

ord-8f88d73a3f4447a087445e19ee915977

반응 방정식

CNCCO
2-(methylamino)ethanol
O=C(Cl)c1ccco1
furoyl chloride
CN(CCO)C(=O)c1ccco1
N-(2-hydroxyethyl)-N-methylfuranamide
수율 57.6%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A one liter, three necked flask was equipped with overhead stirrer
  2. 2
    온도The reaction flask was cooled with an ice bath
  3. 3
    세척The dichloromethane was washed with NaCl(aq.)
  4. 4
    추출Next, the NaCl(aq.) layer was extracted with dichloromethane
  5. 5
    건조dried over MgSO4
  6. 6
    기타The dichloromethane was removed with a rotoevaporator

실험 절차

A one liter, three necked flask was equipped with overhead stirrer, nitrogen atmosphere and an addition funnel. The flask was charged with 115 g of 2-(methylamino)ethanol (1.53 mol.) and 500 ml of dichloromethane. The reaction flask was cooled with an ice bath. Next, 100 g of furoyl chloride (0.77 mol.) was slowly added via the addition funnel over 2.5 hours. The dichloromethane was washed with NaCl(aq.). Next, the NaCl(aq.) layer was extracted with dichloromethane and the two dichloromethane layers were combined and dried over MgSO4. The dichloromethane was removed with a rotoevaporator to yield 75 g (44%) of N-(2-hydroxyethyl)-N-methylfuranamide.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05580647uspto-grants-1996_12