反応 #1166472

ord-8f88d73a3f4447a087445e19ee915977

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A one liter, three necked flask was equipped with overhead stirrer
  2. 2
    温度The reaction flask was cooled with an ice bath
  3. 3
    洗浄The dichloromethane was washed with NaCl(aq.)
  4. 4
    抽出Next, the NaCl(aq.) layer was extracted with dichloromethane
  5. 5
    乾燥dried over MgSO4
  6. 6
    その他The dichloromethane was removed with a rotoevaporator

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05580647uspto-grants-1996_12