HRID251802

反应详情

EQUATION

反应方程式

HRID 251802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of isoquinoline-5-sulfonylchloride hydrochloride (3.00 g, 11.4 mmol) in anhydrous methylene chloride (100 mL) was added tert-butyl 1-homopiperazine carboxylate (3.00 g, 15.0 mmol) and triethylamine (4.36 g, 43.1 mmol). The mixture was stirred for 3 h, evaporated to dryness, mixed with a saturated solution of sodium bicarbonate (100 mL) and extracted with ethyl acetate (80 mL×2). The combined extracts were dried, filtered and evaporated to give an oil (4.45 g, 100%). LCMS (+APCI) m/z 392 (M+H).

WORKUP

后处理

  1. customevaporated to dryness
  2. additionmixed with a saturated solution of sodium bicarbonate (100 mL)
  3. extractionextracted with ethyl acetate (80 mL×2)
  4. customThe combined extracts were dried
  5. filtrationfiltered
  6. customevaporated