HRID1094521
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe title compound is prepared
- temperaturethe resulting yellow solution is heated to and
- temperatureunder reflux for 12 h
- concentrationAfter completion, the reaction mixture is concentrated
- customthe resulting crude product is purified by flash chromatography (SiO2, 100% CH2Cl2)