HRID2102381

反应详情

EQUATION

反应方程式

HRID 2102381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

Methyl 5-{4-[5-(4-fluorophenyl)thieno[2,3-d]pyrimidin-4-yl]butoxy}nicotinate (0.015 g, 0.034 mmol) and ammonia (3.00 mL, 20%, 0.02 mol) were mixed in 1-butanol (1.00 mL) and the resulting mixture was heated at 180° C. for 20 h. The solvent was removed by evaporation, and the product was purified by preparative HPLC to give 5 mg (36%) 5-{4-[5-(4-fluorophenyl)thieno[2,3-d]pyrimidin-4-yl]butoxy}nicotinamide hydroformate as a white solid. MS [M+H]=423.1, LC/MS (EI) tR 3.45 min (Method D), 1H NMR (7% MeOD/CDCl3) δ (ppm) 8.92 (s, 1H), 8.50 (s, 1H), 8.25 (s, 1H), 7.62 (s, 1H), 7.40-7.30 (m, 3H), 7.10 (t, J=8.4 Hz, 2H), 3.84 (t, J=6.0 Hz, 2H), 2.66 (t, J=7.5 Hz, 2H), 1.75-1.58 (m, 2H), 1.59-1.45 (m, 2H).

WORKUP

后处理

  1. customThe solvent was removed by evaporation
  2. customthe product was purified by preparative HPLC