反応 #60588

反応方程式

2-benzoyl-4-benzylmorpholine

chloroformic acid 1-chloromethyl ester

→

2-benzoylmorpholine hydrochloride

収率 67.0%

溶媒

1,2-dichloroethane

反応条件

後処理

1. 1
   濃縮The reaction mixture was concentrated under reduced pressure
2. 2
   workup.DISSOLUTIONThe residue was dissolved in methanol (10 ml)
3. 3
   温度The solution was refluxed for 1 h
4. 4
   濃縮concentrated under reduced pressure
5. 5
   その他The crude product was crystallized from ethyl acetate
6. 6
   ろ過filtrated

実験手順

A solution of 2-benzoyl-4-benzylmorpholine (600 mg, 2.13 mmol) and chloroformic acid 1-chloromethyl ester (457 mg, 3.20 mmol) in 1,2-dichloroethane (8.0 ml) was refluxed for 1 h. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in methanol (10 ml). The solution was refluxed for 1 h and concentrated under reduced pressure. The crude product was crystallized from ethyl acetate and filtrated to give 2-benzoylmorpholine hydrochloride (323 mg, 67%) as a colorless crystal.

出典