HRID1368864
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- dissolutionThe solid partly dissolved
- temperatureThe mixture was heated
- temperatureto near reflux
- customto give a clear dark yellow-green solution
- customThe product crystallized rapidly
- customwas collected after ice-
- temperaturecooling for 1 hour
- washwashed with ice-cold 2-propanol
- customdried in air at 50% relative humidity