HRID594358

反应详情

EQUATION

反应方程式

HRID 594358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A cooled (0° C.) solution of ethyl 4-(1,1-dimethylethylsulfinamido)-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate (1.550 g; 4.00 mmol) in EtOH (20 ml) was treated dropwise with a solution of 4 M HCl in 1,4-dioxane (2.0 ml; 8.00 mmol). The resulting mixture was further stirred at 0° C., under nitrogen, for 10 min., and then at rt for 30 min. The reaction mixture was then concentrated to dryness under reduced pressure and the oily residue was further dried under HV to give the chlorhydrate salt of ethyl 4-amino-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate. LC-MS (conditions A): tR=0.55 min. and [M+H]+: 284.07 g/mol; tR=0.57 min. and [M+H]+: 284.07 g/mol (mixture of diastereoisomers).

WORKUP

后处理

  1. waitat rt for 30 min
  2. concentrationThe reaction mixture was then concentrated to dryness under reduced pressure
  3. customthe oily residue was further dried under HV