HRID471280

反应详情

EQUATION

反应方程式

HRID 471280 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 6-benzyl-1-oxa-6-azaspiro[2.5]octane (2 g) and 2-methylprop-2-en-1-amine HCl (2 g) and Hunig's Base (3.44 mL) in ethanol (30 mL) was heated at 70° C. for 18 hours. The mixture was cooled to room temperature and the solvent evaporated under reduced pressure. The residue was partitioned between DCM and brine, the aqueous layer was re-extracted with fresh DCM and the combined organics dried over sodium sulphate, filtered and the solvent evaporated under reduced pressure to afford the subtitled compound. Yield 2.70 g.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. customthe solvent evaporated under reduced pressure
  3. customThe residue was partitioned between DCM and brine
  4. extractionthe aqueous layer was re-extracted with fresh DCM
  5. dry with materialthe combined organics dried over sodium sulphate
  6. filtrationfiltered
  7. customthe solvent evaporated under reduced pressure