反応 #2799

ord-76b9fb90e765478eb9f07bde4c5ac1d8

反応方程式

O=C(Cl)CCl
chloroacetyl chloride
CN1CCOCC1
N-methylmorpholine
C1COCCN1
morpholine
NC(=O)N1CCOCC1.O=C(O)CCl
chloroacetic acid morpholine carboxamide

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度Cool in an ice-bath
  2. 2
    抽出Extract with cold aqueous 5% sulfuric acid solution, saturated aqueous sodium bicarbonate solution, and saturated aqueous sodium chloride solution
  3. 3
    乾燥Dry the organic layer over Na2SO4
  4. 4
    ろ過filter
  5. 5
    その他evaporate in vacuo

実験手順

Combine chloroacetyl chloride (2.00 mL, 25.0 mmol) and N-methylmorpholine (2.76 mL, 25.0 mmol) in dichloromethane (100 mL). Cool in an ice-bath. Add morpholine (2.19 mL, 25.0 mmol) and stir in the ice-bath for 1 hour. Warm to ambient temperature and stir for 1 hour. Extract with cold aqueous 5% sulfuric acid solution, saturated aqueous sodium bicarbonate solution, and saturated aqueous sodium chloride solution. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to obtain chloroacetic acid morpholine carboxamide.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05731306uspto-grants-1998_03