HRID1295560

反应详情

EQUATION

反应方程式

HRID 1295560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl 4-(4-methanesulfonyl-3,4-dihydro-2H-benzo[1,4]oxazin-6-ylmethyl)piperazine-1-carboxylate (2.5 g, 6.1 mmol) was dissolved in dichloromethane (50 mL) and treated with trifluoroacetic acid (182 mmol). The resulting mixture was stirred at ambient temperature for 3 h then evaporated to dryness under reduced pressure. The residue was extracted with hot ethanol and the combined extracts evaporated to dryness under reduced pressure. Chromatography on SiO2, eluting with 0.880 ammonia/methanol/dichloromethane (1:9:90), gave the title compound (1.2 g, 63%) as an off-white solid.

WORKUP

后处理

  1. customthen evaporated to dryness under reduced pressure
  2. extractionThe residue was extracted with hot ethanol
  3. customthe combined extracts evaporated to dryness under reduced pressure
  4. washChromatography on SiO2, eluting with 0.880 ammonia/methanol/dichloromethane (1:9:90)