HRID1368864

反应详情

EQUATION

反应方程式

HRID 1368864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 5 g of trimetrexate hydrate in 30 ml of 2-propanol and 15 ml of water was added 2.10 g of trifluoroacetic acid (approximately a 40% excess). The solid partly dissolved, but new crystals came out before it was completely gone. The mixture was heated to near reflux to give a clear dark yellow-green solution. To this was added 100 ml of 2-propanol. The product crystallized rapidly, and was collected after ice-cooling for 1 hour, washed with ice-cold 2-propanol and dried in air at 50% relative humidity to give 5.95 g of greenish-yellow crystals.

WORKUP

后处理

  1. dissolutionThe solid partly dissolved
  2. temperatureThe mixture was heated
  3. temperatureto near reflux
  4. customto give a clear dark yellow-green solution
  5. customThe product crystallized rapidly
  6. customwas collected after ice-
  7. temperaturecooling for 1 hour
  8. washwashed with ice-cold 2-propanol
  9. customdried in air at 50% relative humidity