HRID23633

反应详情

EQUATION

反应方程式

HRID 23633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-(4-fluorobenzyl)-2-(chloromethyl)-3,4-dimethyl-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide (104 mg, 0.275 mmol), (1R)-2-(methylamino)-1-pyrazin-2-ylethanol (Preparation 80, 65 mg, 0.0.42 mmol) and diisopropylethylamine (72 μL, 0.0.41 mmol) in dry DMF (5.5 mL) was stirred at room temperature for 17 hours. The solution was then diluted with water (20 mL). The resulting precipitate was collected by filtration and the collected solid was dried in vacuo, providing a white solid. Attempted recrystallization from acetonitrile (20 mL, dissolved with warming and then cooled to room temperature) gave the title compound (31 mg) as a white solid upon concentrating the filtrate.

WORKUP

后处理

  1. filtrationThe resulting precipitate was collected by filtration
  2. customthe collected solid was dried in vacuo
  3. customproviding a white solid
  4. customAttempted recrystallization from acetonitrile (20 mL
  5. dissolutiondissolved
  6. temperaturewith warming
  7. temperaturecooled to room temperature)