HRID1043880

反应详情

EQUATION

反应方程式

HRID 1043880 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Methylhydrazine (3.94 mL) was added dropwise to a solution of (S)-t-butyl (1,3-dioxoisoindolin-2-yl)(tetrahydrofuran-3-yl)carbamate (12.3 g) in THF (125 mL) under ice-cooling over two minutes. The reaction mixture was stirred at 0° C. for 30 minutes, at room temperature for three days and then at 50° C. for four hours. The reaction mixture was ice-cooled, and the insoluble matter was then removed from the reaction mixture by filtration. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 10% to 14%) to give the title compound (7.04 g).

WORKUP

后处理

  1. temperaturecooling over two minutes
  2. waitat 50° C. for four hours
  3. temperaturecooled
  4. customthe insoluble matter was then removed from the reaction mixture by filtration
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 10% to 14%)