HRID630035

反应详情

EQUATION

反应方程式

HRID 630035 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(bromomethyl)-1-methyl-benzimidazole hydrobromide (6.8 mmol), 6-methyl-2-sulfanylpyrimidin-4-ol (740 mg, 5.2 mmol), and triethylamine (4 mL, 28.7 mmol) in absolute ethanol (30 mL) was stirred at room temperature overnight. The mixture was recovered, evaporated, and then co-evaporated with EtOAc (20 mL). The solid residue was treated with water (200 mL). The solid product was recovered by filtration, washed with water (2×20 mL), diethyl ether (2×20 mL), and hexanes (2×20 mL), and then dried in vacuo, affording 6-methyl-2-{[(1-methyl-1H-benzimidazol-2-yl)methyl]sulfanyl}pyrimidin-4-ol (1.3 g, 90% yield); 1H NMR (400 MHz, DMSO-d6): δ 2.18 (s, 3H), 3.83 (s, 3H), 4.70 (s, 2H), 6.02 (s, 1H), 7.19 (m, 2H), 7.53 (m, 2H); M+287. The product was used without further purification.

WORKUP

后处理

  1. customThe mixture was recovered
  2. customevaporated
  3. additionThe solid residue was treated with water (200 mL)
  4. filtrationThe solid product was recovered by filtration
  5. washwashed with water (2×20 mL), diethyl ether (2×20 mL), and hexanes (2×20 mL)
  6. customdried in vacuo