HRID82872

反应详情

EQUATION

反应方程式

HRID 82872 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
210 °C

PROCEDURE

实验过程

N-((7-Amino-8-benzyl-5,6,7,8-tetrahydronaphthalen-2-yl)methyl)ethanesulfonamide (0.243 g, 0.678 mmol) and 3-oxetanone (0.098 g, 1.356 mmol) were sealed in a vial and heated at 210° C. for 2 minutes. Trimethylsilyl cyanide (0.181 mL, 1.356 mmol) was added, the vial was resealed and the mixture was heated again at 210° C. for 2 minutes. The mixture was diluted with ethyl acetate (40 mL) and washed with 1 N NaOH (1×20 mL) and brine (1×20 mL). The organic extract was collected, dried on MgSO4 and evaporated under reduced pressure to give a brown oil. The residue was purified by preparative HPLC. Product was obtained as a colourless oil (7.2 mg, 0.016 mmol, 2.4%).

WORKUP

后处理

  1. temperaturethe mixture was heated again at 210° C. for 2 minutes
  2. washwashed with 1 N NaOH (1×20 mL) and brine (1×20 mL)
  3. extractionThe organic extract
  4. customwas collected
  5. customdried on MgSO4
  6. customevaporated under reduced pressure
  7. customto give a brown oil
  8. customThe residue was purified by preparative HPLC