HRID1094521

反应详情

EQUATION

反应方程式

HRID 1094521 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound is prepared according to a published literature procedure (see J. Med. Chem. 2002, 45, 2994-3008.): 4.17 g (32.3 mMol) of pivaloylacetonitrile are added to a solution of 4.20 g (32.3 mMol) 4-fluoro-phenylhydrazine in 150 ml of toluene at rt, and the resulting yellow solution is heated to and kept under reflux for 12 h. After completion, the reaction mixture is concentrated, and the resulting crude product is purified by flash chromatography (SiO2, 100% CH2Cl2) to give the title compound as a yellow solid: 1HNMR (CDCl3) δ ppm 7.59 (d, 2H), 7.10 (d, 2H), 5.58 (s, 1H), 3.62 (brs, H2N), 1.32 (s, 9H).

WORKUP

后处理

  1. customThe title compound is prepared
  2. temperaturethe resulting yellow solution is heated to and
  3. temperatureunder reflux for 12 h
  4. concentrationAfter completion, the reaction mixture is concentrated
  5. customthe resulting crude product is purified by flash chromatography (SiO2, 100% CH2Cl2)