HRID1449536

反应详情

EQUATION

反应方程式

HRID 1449536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 4-hydroxy-1,1-dioxo-1,2-dihydro-1λ6 -benzo[e][1,2]thiazine-3-carboxylic acid methyl ester (1.48 g, 5.84 mmol) in DMF (10 mL) was added sodium hydride (0.257 g, 60%, 6.4 mmol) and the mixture stirred for 5 minutes. 3,4-methylenedioxybenzyl chloride (2.2 g, 50 wt. % in dichloromethane, 6.4 mmol) was added and the mixture stirred at room temperature for 18 hours. Diluted with ethyl acetate (100 mL), washed with water (2×80 mL), brine (80 mL), dried over magnesium sulfate, removed solvent in vacuo, and crystallized from ethyl acetate/heptane to give the title compound (1.63 g, 72%);

WORKUP

后处理

  1. stirringthe mixture stirred at room temperature for 18 hours
  2. washwashed with water (2×80 mL), brine (80 mL)
  3. dry with materialdried over magnesium sulfate
  4. customremoved solvent in vacuo
  5. customcrystallized from ethyl acetate/heptane