HRID660426

反应详情

EQUATION

反应方程式

HRID 660426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

{1-Benzyl-3-[(3-fluoro-4-nitro-benzenesulfonyl)-isobutyl-amino]-2-hydroxy-propyl}-carbamic acid hexahydro-furo[2,3-b]furan-3-yl ester (7) (0.40 g, 0.67 mmol, 1 equiv) and 2,4-difluoro-benzylamine (0.14 g, 1 mmol, 1.49 equiv) were dissolved in tetrahydrofurane (10 mL). The solution was heated to reflux for 18 h. The solution was concentrated and the crude product was dissolved in dichloromethane (15 mL). The organic layer was washed with saturated NaHCO3 solution (15 mL). The organic layer was separated and evaporated under reduced pressure to yield the title compound (0.48 g, 0.67 mmol, quantitative). LRMS (ES+): m/z 719 [M+H]+.

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureto reflux for 18 h
  3. concentrationThe solution was concentrated
  4. dissolutionthe crude product was dissolved in dichloromethane (15 mL)
  5. washThe organic layer was washed with saturated NaHCO3 solution (15 mL)
  6. customThe organic layer was separated
  7. customevaporated under reduced pressure