HRID1603309

反应详情

EQUATION

反应方程式

HRID 1603309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

--Quantities bromopyrimidine 16 (3.72 g, 8.25 mmol), 1.6M butyllithium (5.7 ml, 9.1 mmol), trimethyl borate (1.9 ml, 16.5 mmol), THF (80 ml), 30% hydrogen peroxide (3.7 ml, 33 mmol). The experimental procedure was as described for compound 33. The crude product was purified by flash chromatography (10 to 30% ethyl acetate-light petroleum) to give the hydroxypyrimidine 48 (1.82 g, 57%) (from MeOH), m.p. 157.3° C.; νmax /cm-1 (KBr) 2920, 2720, 2580, 1505, 1430, 1280, 1240 and 1180 δ 0.85 (7H, m), 1.05-1.38 (10H, m), 1.50 (2H, m), 1.73 (4H, t), 2.68 (2 H, t, ArCH2), 7.01 (1H, ddd, 5'-H), 7.55 (1H, ddd, 6'-H), 8.37 (2H, s, 4- and 6-H) and 9.7 (1H, br s); m/z 388 (M+), 317 (M+ -C5H11), 235, 222 and 204.

WORKUP

后处理

  1. customThe crude product was purified by flash chromatography (10 to 30% ethyl acetate-light petroleum)