HRID405954

反应详情

EQUATION

反应方程式

HRID 405954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixture of 3-bromo-2-(chloromethyl)-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (4.5322 g, 15.76 mmol), potassium acetate (2.320 g, 23.64 mmol), and DMF (60.0 mL) was stirred at 40° C. After 3.5 h, the mixture was concd under reduced pressure. To the residue was added water (100 mL) and the resulting precipitate was collected by filtration, washed with water (100 mL), and dried to give (3-bromo-6-methyl-4-oxo-4H-pyrido[1,2-a]pyrimidin-2-yl)methyl acetate as a brown solid: 1H NMR (400 MHz, DMSO-d6) δ ppm 7.75 (1 H, dd, J=9.0, 7.0 Hz), 7.45 (1 H, dd, J=9.0, 0.8 Hz), 7.02-7.08 (1 H, m), 5.12 (2H, s), 2.95 (3 H, s), 2.14 (3 H, s); Mass Spectrum (ESI) m/e=310.9 [M+1 (79Br)] and 313.0 [M+1 (81Br)].

WORKUP

后处理

  1. filtrationthe resulting precipitate was collected by filtration
  2. washwashed with water (100 mL)
  3. customdried