HRID1455584

反应详情

EQUATION

反应方程式

HRID 1455584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of (3) (1.5 g, 4.3 mmol) in diglyme is heated at 150° C. in a microwave reactor (Smith Creator, S00219) for 40 minutes. Solvent evaporated under vacuum in Genevac Evaporator at 80° C. for 3hours to give a solid. This is taken in dichloromethane (40 mL) and treated with trifluoroacetic acid at room temperature for 2 hours. Solvent evaporated to dryness under reduced pressure, crude taken in water, washed with DCM, aqueous layer basified with 1M NaOH solution and extracted with dichloromethane. Organic layer dried over Na2SO4 and evaporated under reduced pressure to give 2-amino-1-(5-phenyl-[1,2,4]oxadiazol-3-yl)-butan-1-ol (300 mg) as a solid.

WORKUP

后处理

  1. customSolvent evaporated under vacuum in Genevac Evaporator at 80° C. for 3hours
  2. customto give a solid
  3. customSolvent evaporated to dryness under reduced pressure, crude
  4. washwashed with DCM, aqueous layer
  5. extractionextracted with dichloromethane
  6. dry with materialOrganic layer dried over Na2SO4
  7. customevaporated under reduced pressure