HRID347457

反应详情

EQUATION

反应方程式

HRID 347457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 1-(3-fluoro-4-hydroxyphenyl)-3-(2-(4-fluorophenyl)acetyl)thiourea (24 mg, 0.075 mmol), 4,6-dichloro-1-methyl-1H-pyrazolo[3,4-d]pyrimidine (15.3 mg, 0.075 mmol, preparation: J. Org. Chem. 1958, 23, 852, the disclosure of which is herein incorporated by reference) and K2CO3 (10 mg, 0.075 mmol) was added DMF (2 mL). The reaction was stirred at RT for 24 h. The reaction was quenched with water (2 mL) and CH2Cl2 (5 mL). The organic layer was separated, dried with sodium sulfate, concentrated in vacuo and purified by reverse phase preparative HPLC to give the title compound (22.9 mg, 60%) as a white solid. MS(ESI+) m/z 457 (M+H)+.

WORKUP

后处理

  1. custom15.3 mg, 0.075 mmol, preparation
  2. customThe reaction was quenched with water (2 mL) and CH2Cl2 (5 mL)
  3. customThe organic layer was separated
  4. dry with materialdried with sodium sulfate
  5. concentrationconcentrated in vacuo
  6. custompurified by reverse phase preparative HPLC