HRID1882579
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
6-(2,2-Diphenyl-ethylamino)-9H-purine-2-carboxylic acid methyl ester hydrochloride (prepared using the procedure described in international patent application WO 2001/94368) (35 g, 85.3 mmol) is placed in a flask under an atmosphere of argon. Dry CHCl3 (300 ml) and N,O-bis(trimethylsilyl)acetamide (61 ml) are added and the reaction mixture is refluxed for 1 hour. The reaction mixture is allowed to cool and any volatiles removed in vacuo. To the resulting oil is added MeOH (300 ml). The resulting white solid is filtered and washed with MeOH (2×200 ml) and then dried in a vacuum oven to give the title compound. 1H NMR (DMSO, 400 MHz).
WORKUP
后处理
- customis placed in a flask under an atmosphere of argon
- temperaturethe reaction mixture is refluxed for 1 hour
- temperatureto cool
- customany volatiles removed in vacuo
- additionTo the resulting oil is added MeOH (300 ml)
- filtrationThe resulting white solid is filtered
- washwashed with MeOH (2×200 ml)
- customdried in a vacuum oven