HRID1433074

反应详情

EQUATION

反应方程式

HRID 1433074 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the suspension of 2-[4-(6-chloro-benzo[b]thiophene-2-sulfonyl)-2-oxo-piperazin-1-ylmethyl]-6,7-dihydro-5H-benzothiazol-4-one (7 mg, 0.01 mmol) in EtOH (1 mL) is added sodium borohydride (3 mg, 0.08 mmol). After 15 min the reaction is diluted with EtOAc and washed with 1N HCl, NaHCO3 and brine. The solution is dried (MgSO4) and concentrated to provide 4-(6-chloro-benzo[b]thiophene-2-sulfonyl)-1-(4-hydroxy-4,5,6,7-tetrahydro-benzothiazol-2-ylmethyl)-piperazin-2-one. 1H NMR (300 MHz, CDCl3) δ 7.88-7.82 (m, 3H), 7.46 (dd, 1H), 4.83-4.81 (m, 1H), 4.76 (s, 1H), 4.75 (s, 1H), 3.92 (s, 1H), 3.91 (s, 1H), 3.62-3.55 (m, 2H), 3.47-3.41 (m, 2H), 2.76-2.62 (m, 2H), 2.05-1.78 (m, 4H); MS (Ion Spray) 498 (M+H)+.

WORKUP

后处理

  1. washwashed with 1N HCl, NaHCO3 and brine
  2. dry with materialThe solution is dried (MgSO4)
  3. concentrationconcentrated