HRID1802320

反应详情

EQUATION

反应方程式

HRID 1802320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 14-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-N-(2,5-dimethylphenyl)-1-piperidinecarbothioamide (i.e. the product of Step C) (476 mg, 1.0 mmol) and methyl iodide (0.25 mL, 4.0 mmol) in dichloromethane (2 mL) was agitated at room temperature for 3 h. The reaction mixture was then diluted with dichloromethane, washed with saturated aqueous sodium bicarbonate, saturated aqueous sodium chloride, dried (MgSO4), and concentrated to give a foamy white solid (480 mg). The solid was crystallized from methyl acetate/petroleum ether to give the title compound, a compound of the present invention, as a white powder (320 mg) melting at 114-116° C.

WORKUP

后处理

  1. washwashed with saturated aqueous sodium bicarbonate, saturated aqueous sodium chloride
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated