HRID720613

反应详情

EQUATION

反应方程式

HRID 720613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAt this time, the reaction was cooled to 0° C.
  2. filtrationfiltered
  3. washwashed with water