HRID1172601

反应详情

EQUATION

反应方程式

HRID 1172601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

In an inert atmosphere, 1-ethyl-3-methyl-4-[2-(4-trifluoromethyl-phenyl)-ethyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine (51 mg, 0.15 mmol) was dissolved in 3-methyl-2-butyl-ketone (MIBK) (1 ml) followed by the addition of DIPEA (21.3 mg, 0.165 mmol) and toluene-4-sulfonic acid methylcarbamoyl-phenyl-methyl ester (71.8 mg, 0.225 mmol). The reaction mixture was heated to 90° C. for 24 h, concentrated in vacuo and the crude product was purified by prep. HPLC to give 70 mg (95%) of 2-{1-ethyl-3-methyl-4-[2-(4-trifluoromethyl-phenyl)-ethyl]-1,4,6,7-tetrahydro-pyrazolo[4,3-c]pyridin-5-yl}-N-methyl-2-phenyl-acetamide. LC-MS: tR=0.84 min; [M+H]+=485.28.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. customthe crude product was purified by prep