HRID1918210

反应详情

EQUATION

反应方程式

HRID 1918210 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10% Pd/C (13.7 mg, 13 μmol, 20 mol % Pd) was added to methyl 4-(benzyloxycarbonylamino)-2-(4-chlorophenyl)-5-bromothiophene-3-carboxylate (6) (31.0 mg, 64 μmol) in ethanol:ethyl acetate:dichloromethane (2:1:1, 2.0 mL). The mixture was degassed and placed under H2 (1 atm) and stirred for 4 h. The mixture was filtered through a 0.45 μm syringe filter and concentrated under reduced pressure. Flash chromatography (ISCO system, silica, 0-50% ethyl acetate in hexane) provided 7 (16.6 mg, 64%) as a solid: LRESIMS m/z 401.9 [M+H]+, calcd. for C20H17Cl1N1O4S1 402.6.

WORKUP

后处理

  1. customThe mixture was degassed
  2. filtrationThe mixture was filtered through a 0.45 μm syringe
  3. filtrationfilter
  4. concentrationconcentrated under reduced pressure