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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
A solution of 2-(4-acetylamino-phenyl)-N-[6-amino-3-(2-fluoro-benzyl)-2,4-dioxo-1-(1-trityl-1H-[1,2,4]triazol-3-ylmethyl)-1,2,3,4-tetrahydro-pyrimidin-5-yl]-acetamide (50 mg, 0.06 mmol) in methanol (2.0 mL) was treated with a 10% aqueous sodium hydroxide solution (0.8 mL). The reaction was heated to 50° C. for 8 h. At this time, the reaction was cooled to 0° C., acidified with a 3N aqueous hydrochloric acid solution, filtered, and washed with water to afford N-{4-[1-(2-fluoro-benzyl)-2,6-dioxo-3-(1-trityl-1H-[1,2,4]triazol-3-ylmethyl)-2,3,6,7-tetrahydro-1H-purin-8-ylmethyl]-phenyl}-acetamide (36 mg, 75%) as an off-white solid: 1H NMR (DMSO-d6, 300 MHz) δ13.45 (broad s, 1H), 9.87 (s, 1H), 7.94 (s, 1H), 7.47–6.89 (m, 23H), 5.21 (s, 2H), 5.07 (s, 2H), 3.95 (s, 2H), 2.48 (s, 3H).
WORKUP
后处理
- temperatureAt this time, the reaction was cooled to 0° C.
- filtrationfiltered
- washwashed with water