2-(Methylamino)ethanol → N-(2-hydroxyethyl)-N-methylfuranamide

HRID 259664

반응식

HRID 259664 반응식
[CH3:1][NH:2][CH2:3][CH2:4][OH:5].[O:6]1[CH:10]=[CH:9][CH:8]=[C:7]1[C:11](Cl)=[O:12]>ClCCl>[OH:5][CH2:4][CH2:3][N:2]([CH3:1])[C:11]([C:7]1[O:6][CH:10]=[CH:9][CH:8]=1)=[O:12]

참가 물질

4

반응물 2

HCID 80162-(Methylamino)ethanolHCID 682422-Furancarbonyl chloride

생성물 1

HCID 15134402N-(2-hydroxyethyl)-N-methylfuranamide수율 57.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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.

후처리

  1. customA one liter, three necked flask was equipped with overhead stirrer
  2. temperatureThe reaction flask was cooled with an ice bath
  3. washThe dichloromethane was washed with NaCl(aq.)
  4. extractionNext, the NaCl(aq.) layer was extracted with dichloromethane
  5. dry with materialdried over MgSO4
  6. customThe dichloromethane was removed with a rotoevaporator

출처 및 근거

ORD 기록
ord-7e06603def354335a124d1172e350dc5
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05523152

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