HRID919781

反应详情

EQUATION

反应方程式

HRID 919781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A flask was charged with 3-methyl-6-oxo-1,6-dihydro-pyridine-2-carboxylic acid ethyl ester (230 mg, 1.27 mmol), toluene (6.4 mL) and water (0.064 mL). K2CO3 (351 mg, 2.54 mmol), LiBr (221 mg, 2.54 mmol), tetrabutylammonium bromide (41 mg, 0.127 mmol), and benzyl bromide (0.23 mL, 1.91 mmol) were added, and the resulting suspension was heated at 80° C. for 40 min. The mixture was allowed to come to r.t., diluted with CH2Cl2, and filtered. The filtrate was concentrated in vacuo, and the residue was chromatographed (0-10% MeOH/CH2Cl2) to give 158 mg of the title compound as a viscous oil. MS: (+) m/z 272.31 (M+1).

WORKUP

后处理

  1. customto come to r.t.
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated in vacuo
  4. customthe residue was chromatographed (0-10% MeOH/CH2Cl2)