HRID56396

反应详情

EQUATION

反应方程式

HRID 56396 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Tert-butyl ((3R,4S)-4-(1,3-dioxoisoindolin-2-yl)tetrahydrofuran-3-yl)carbamate (13.08 g, 39.4 mmol) was dissolved into ethanol (98 mL, 0.4 M)). Hydrazine monohydrate (1.97 g, 39.4 mmol) was added, and the reaction was stirred 30 minutes at 50° C. and then 2 hours at 75° C. The reaction was then cooled to room temperature and the white solid was removed by filtration. The filtrate was concentrated down and dried, then treated with ethanol (about 15 mL). Additional white solid was removed by filtration, then filtrate was concentrated down and dried to yield tert-butyl ((3R,4S)-4-aminotetrahydrofuran-3-yl)carbamate as a thick, clear oil (8.724 g at 90% purity; 99%).

WORKUP

后处理

  1. custom2 hours
  2. customat 75° C
  3. temperatureThe reaction was then cooled to room temperature
  4. customthe white solid was removed by filtration
  5. concentrationThe filtrate was concentrated down
  6. customdried
  7. additiontreated with ethanol (about 15 mL)
  8. customAdditional white solid was removed by filtration
  9. concentrationfiltrate was concentrated down
  10. customdried