HRID1376197

反应详情

EQUATION

反应方程式

HRID 1376197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

3.3 g of 1-(9-Benzenesulfonyl-9H-carbazol-4-yloxy)-3-{benzyl-[2-(2-methoxy-phenoxy)-ethyl]-amino}-propan-2-ol (5.2 mmol) were dissolved in 33 ml THF/methanol (2:1). A solution of 1.1 g of sodium hydroxide in 1.7 ml of water was added in one portion. The mixture was stirred for 18 h at 50° C. The mixture was rotary evaporated (35° C./20 mbar). The residue was dissolved in 25 ml of toluene and 20 ml of water. The phases were separated and the toluene phase was washed 3 times with 25 ml of water. The organic phase was rotary evaporated (40° C./15 mbar) and the residue was crystallized with 9 ml ethanol. The product was filtered under suction and washed twice with 3 ml cold ethanol. The substance was dried at 50° C. for 12 h.

WORKUP

后处理

  1. customThe mixture was rotary evaporated (35° C./20 mbar)
  2. dissolutionThe residue was dissolved in 25 ml of toluene
  3. customThe phases were separated
  4. washthe toluene phase was washed 3 times with 25 ml of water
  5. customThe organic phase was rotary evaporated (40° C./15 mbar)
  6. customthe residue was crystallized with 9 ml ethanol
  7. filtrationThe product was filtered under suction
  8. washwashed twice with 3 ml cold ethanol
  9. customThe substance was dried at 50° C. for 12 h.