HRID913040

反应详情

EQUATION

反应方程式

HRID 913040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 3-benzyloxy-6-methyl-4-oxo-1,4-dihydro-pyridine-2-carboxylic acid (5.2 g, 20.0 mmol) in dimethylformamide (12 mL) was heated in an oil bath for 8 h. The temperature of the oil bath was maintained at 120° C. A solid separated upon cooling to RT. The solid 5-benzyloxy-2-methyl-1H-pyridin-4-one was suction filtered and washed with hexane. The isolated solid was dried under high vacuum for 16 h (3.32 g, 77% yield). 1H NMR (400 MHz, MeOH-D4) δ (ppm): 7.45-7.46 (m, overlapping peaks, 2H, Ar—H and CH), 7.29-7.39 (m, overlapping peaks, 4H, Ar—H), 6.34 (s, 1H, CH), 5.07 (s, 2H, OCH2), 2.30 (s, 3H, CH3); MS-ESI (m/z): 216.3 [M+1]+, 215.6 [M]+, 188.3.

WORKUP

后处理

  1. temperaturewas heated in an oil bath for 8 h
  2. customA solid separated
  3. temperatureupon cooling to RT
  4. filtrationfiltered
  5. washwashed with hexane
  6. customThe isolated solid was dried under high vacuum for 16 h (3.32 g, 77% yield)