HRID1259465

反应详情

EQUATION

反应方程式

HRID 1259465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(2S)-2-[(benzylamino)methyl]-2,3,8,9-tetrahydro-7H-[1,4]dioxino[2,3-e]indol-8-one 4-methylbenzenesulfonate (0.75 g, 1.54 mmol) is suspended in 2-methyl tetrahydrofuran (10 mL), 1 N NaOH is added until the solids dissolve and the pH of the aqueous phase is 10 (pH paper), about 1.6 mL is required. The aqueous layer is removed, and the organic phase is washed with water (2×2 mL). The volatiles are removed by rotary evaporation to give a yellow syrup. The syrup is dissolved in absolute ethanol (3 mL) and evaporated to dryness. Absolute ethanol (3 mL) is added to the residue and removed by rotary evaporation to give crude (2S)-2-[(benzylamino)methyl]-2,3,8,9-tetrahydro-7H-[1,4]dioxino[2,3-e]indol-8-one as a yellow syrup which is carried directly into the next step.

WORKUP

后处理

  1. dissolutiondissolve
  2. customThe aqueous layer is removed
  3. washthe organic phase is washed with water (2×2 mL)
  4. customThe volatiles are removed by rotary evaporation
  5. customto give a yellow syrup
  6. customevaporated to dryness
  7. additionAbsolute ethanol (3 mL) is added to the residue
  8. customremoved by rotary evaporation