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

HRID 1079290

反応式

HRID 1079290 の反応式
[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]

参加物

4

反応物 2

HCID 80162-(Methylamino)ethanolHCID 682422-Furancarbonyl chloride

生成物 1

HCID 15134402N-(2-hydroxyethyl)-N-methylfuranamide収率 57.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8f88d73a3f4447a087445e19ee915977
出典データセット
uspto-grants-1996_12
特許番号
US05580647

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