HRID517765

反应详情

EQUATION

反应方程式

HRID 517765 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a solution of 5-(chloromethyl)-1-[3-(trifluoromethyl)phenyl]-1H-tetrazole (80 mg, 0.305 mmol, commercially available from Otava, Kiev, Ukraine) in acetonitrile (2 mL) was added 3,3-dimethylmorpholine (46.2 mg, 0.305 mmol, commercially available, for example from Otava, Kiev, Ukraine or Tyger Scientific, Ewing, USA) and triethylamine (0.127 mL, 0.914 mmol). The reaction mixture was then heated to 120° C. for 50 min in a microwave reactor. The reaction mixture was concentrated in vacuo and the crude product was purified by MDAP. The relevant fractions were combined and concentrated in vacuo. The product was dissolved in DCM and 1N HCl in ether (110 uL) was added. The mixture was concentrated in vacuo, triturated with ether, then dried in vacuo to yield the title compound (white crystals, 40 mg).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe crude product was purified by MDAP
  3. concentrationconcentrated in vacuo
  4. dissolutionThe product was dissolved in DCM
  5. addition1N HCl in ether (110 uL) was added
  6. concentrationThe mixture was concentrated in vacuo
  7. customtriturated with ether
  8. customdried in vacuo