HRID1812342

反应详情

EQUATION

反应方程式

HRID 1812342 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

The solid 4-(5-(3,6-dihydro-2H-pyran-4-yl)-2-fluoropyridin-3-yl)-N,N-bis(4-methoxybenzyl)-6-methyl-1,3,5-triazin-2-amine (130 mg, 0.246 mmol) from step 1 was dissolved in THF (30 mL) and mixed with palladium hydroxide on carbon (20%, 80 mg). The mixture was purged with hydrogen through vacuum/back-fill (3×) and stirred under a hydrogen balloon. After 15 h, the mixture was heated to about 50° C. for 2 h. The mixture was cooled to room temperature and filtered through a pad of Celite® (diatomaceous earth). The filtrate was concentrated to a yellow film. m/z (ESI, positive ion): 530.2 (M+H)+.

WORKUP

后处理

  1. customThe mixture was purged with hydrogen through vacuum/back-fill (3×)
  2. temperatureThe mixture was cooled to room temperature
  3. filtrationfiltered through a pad of Celite® (diatomaceous earth)
  4. concentrationThe filtrate was concentrated to a yellow film