HRID1044518

反应详情

EQUATION

反应方程式

HRID 1044518 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl [1-(4-chlorobenzyl)-7-{3-[(propylsulfonyl)amino]propyl}-1,2,3,4-tetrahydronaphthalen-2-yl]carbamate (150 mg, 0.281 mmol) was dissolved in dichloromethane (3 mL) and a solution of hydrochloric acid (0.5 mL, 5 M in isopropanol) was added. After stirring at room temperature for 2 hours the solvent was removed in vacuo. Water was added (15 mL) and the pH was adjusted to 9 with aqueous saturated sodium bicarbonate and the mixture was extracted with dichloromethane (3×15 mL). The combined organic extracts were dried and concentrated in vacuo. The crude product was purified by flash chromatography (silica gel, dichloromethane, methanol). The product was dissolved in dichloromethane (2 mL) and a solution of hydrochloric acid in ethanol (1.25 M) was added. The solvent was removed in vacuo. Yield: 31.4 mg (0.187 mmol, 36%).

WORKUP

后处理

  1. customwas removed in vacuo
  2. additionWater was added (15 mL)
  3. extractionthe mixture was extracted with dichloromethane (3×15 mL)
  4. customThe combined organic extracts were dried
  5. concentrationconcentrated in vacuo
  6. customThe crude product was purified by flash chromatography (silica gel, dichloromethane, methanol)
  7. dissolutionThe product was dissolved in dichloromethane (2 mL)
  8. additiona solution of hydrochloric acid in ethanol (1.25 M) was added
  9. customThe solvent was removed in vacuo