HRID589702

反应详情

EQUATION

反应方程式

HRID 589702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-(1H-tetrazol-5-yl)-phenylamine (161 mg, 10 mmol) in dry CH2Cl2 (10 mL) pyridine (0.5 mL) and 3,5-dimethyl-benzothiophene-2-sulfonyl chloride (Intermediate 13) (260 mg, 10 mmol) were added. The mixture was stirred for 4 h and then concentrated in vacuo. The product was purified by column chromatography on silica gel (eluent: 2 to 15% MeOH in CHCl3) affording 104 mg (27%) of the title compound. 1H NMR (DMSO-d6) δ ppm 2.40 (s, 3H) 2.52 (s, 3H) 7.29 (d, 1H) 7.35 (d, 1H) 7.42 (t, 1H) 7.70 (m, 2H) 7.85 (d, 1H) 7.92 (s, 1H). MS (ESI+) calcd for C17H15N5O2S2 385.066716, found 385.065826.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. customThe product was purified by column chromatography on silica gel (eluent: 2 to 15% MeOH in CHCl3)