HRID1789955

反应详情

EQUATION

反应方程式

HRID 1789955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
119 °C

PROCEDURE

实验过程

To ethyl (6bR,10aS)-2,3,6b,9,10,10a-hexahydro-1H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxaline-8(7H)-carboxylate (4.10 g, 14.3 mmol) was added n-butanol (18.0 mL) and KOH powder (3.0 g). The reaction was heated at 119° C. in a sealed tube for 18 hr. The solvent was removed under reduced pressure. To the residue was added water (30 mL) extracted with CH2Cl2 (3×50 mL). The combined organic layers were washed with brine, dried over MgSO4, and concentrated to afford the title compound as a pale yellow oil (2.70 g, 78%). MS-ESI: 216 [MH]+

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. additionTo the residue was added water (30 mL)
  3. extractionextracted with CH2Cl2 (3×50 mL)
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated