HRID1400015

反应详情

EQUATION

反应方程式

HRID 1400015 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Zn powder (5.07 g, 77.6 mmol) was added to a solution of (R,R)-2-methyl-propane-2-sulfinic acid [1-(4-fluoro-phenyl)-2-nitro-ethyl]-amide (2.24 g, 7.76 mmol) and NH4Cl (4.15 g, 77.6 mmol) in 5:1 acetone/H2O (24 mL) at rt. After 10 min, the reaction mixture was filtered and the filtrate concentrated under reduced pressure. The crude residue was crystallized using CH2Cl2 (20 mL) and hexanes (50 mL) to provide (R,R)-2-methyl-propane-2-sulfinic acid [2-amino-1-(4-fluoro-phenyl)-ethyl]-amide (1.8 g, 89%). MS (ESI+): calcd for C12H19FN2OS m/z 258.12. found 259.1 (M+H)+.

WORKUP

后处理

  1. filtrationthe reaction mixture was filtered
  2. concentrationthe filtrate concentrated under reduced pressure
  3. customThe crude residue was crystallized