反応 #690509

反応方程式

ethyl fluoroacetate

morpholine

HCl

→

title compound

収率 74.6%

2-Fluoro-1-morpholin-4-yl-ethanone

収率 74.6%

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度After cooling to ambient temperature
2. 2
   その他The organic layer was separated
3. 3
   抽出the aqueous layer was extracted with dichloromethane (200 mL×2)
4. 4
   乾燥The combined organic phase was dried over anhydrous MgSO4
5. 5
   濃縮concentrated in vacuo

実験手順

A mixture of ethyl fluoroacetate (50 g, 472 mmol) and morpholine (82 g, 944 mmol) was heated at 70° C. for 20 h. After cooling to ambient temperature, the mixture was added to a stirred mixture of 2 N HCl (240 mL) and methylene chloride (200 mL) over 20 min. The organic layer was separated and the aqueous layer was extracted with dichloromethane (200 mL×2). The combined organic phase was dried over anhydrous MgSO4 and concentrated in vacuo to give 51.7 g (74.6%) of the title compound. 1H NMR (400 MHz, CDCl3) δ 4.96 (d, J=47.2 Hz, 2H), 3.70 (bs, 4H), 3.64 (bs, 2H), 3.47 (bs, 2H).

出典