HRID2382115

反应详情

EQUATION

反应方程式

HRID 2382115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

LiAlH4 (14.7 mmol, 1 M solution in THF) is added to a solution of 6-fluoro-4H-benzo[1,4]oxazin-3-one (1.23 g, 7.35 mmol) in THF at rt and heated to reflux for 2 hrs. The reaction mixture is quenched with a few drops of water followed by slow addition of ethyl acetate (10 mL). The solid is filtered off, and washed with EtOAc. The filtrate is concentrated in vacuo to afford 6-fluoro-3,4-dihydro-2H-benzo[1,4]oxazine (1 g). MS: 154 (M+H).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 2 hrs
  3. customThe reaction mixture is quenched with a few drops of water
  4. additionfollowed by slow addition of ethyl acetate (10 mL)
  5. filtrationThe solid is filtered off
  6. washwashed with EtOAc
  7. concentrationThe filtrate is concentrated in vacuo