HRID2235490

反应详情

EQUATION

反应方程式

HRID 2235490 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 0.040 g (0.11 mmol) of 1-[4-(Dipropylamino)pyridin-2-yl]-3-mesitylthiourea in 2 mL of glacial acetic acid was added 6.1 μL (0.12 mmol) of bromine. After 30 min at room temperature, an additional 2 μL of bromine was added. The reaction mixture was concentrated after 2 h and washed with ethyl acetate/hexanes. The organics were concentrated and the resulting oil was purified by flash chromatography eluting with a 4% methanol/dichloromethane mixture to give 0.020 g (50%) of the title compound as a light yellow powder.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated after 2 h
  2. washwashed with ethyl acetate/hexanes
  3. concentrationThe organics were concentrated
  4. customthe resulting oil was purified by flash chromatography
  5. washeluting with a 4% methanol/dichloromethane mixture