HRID247134

反应详情

EQUATION

反应方程式

HRID 247134 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 2,3,3a,4,7,7a-hexahydro-3a-hydroxy-5-methyl-7-(2-nitrophenyl)-1,1-dioxothieno[3,2-b]pyridine-6-carboxylate (2.5 g, 0.0065 moles) and toluene (60 mL) was refluxed for 24 hours. The solvent was removed in vacuo and the resulting solid was recrystallized from ethanol. The crystals were washed with diethyl ether 2× and dried at 65° C. under high vacuum for 48 hours. This gave 1.78 g product; mp 215°-217° C.

WORKUP

后处理

  1. temperaturewas refluxed for 24 hours
  2. customThe solvent was removed in vacuo
  3. customthe resulting solid was recrystallized from ethanol
  4. washThe crystals were washed with diethyl ether 2×
  5. customdried at 65° C. under high vacuum for 48 hours