HRID1401864

反应详情

EQUATION

反应方程式

HRID 1401864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

680 mg (2.19 mmol) of [4-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)thiazol-2-yl]acetonitrile from step a are dissolved in 10 ml of THF, placed under nitrogen, boiled to reflux, and 1.21 ml (2.41 mmol) of a 2M borane dimethyl sulfide complex solution in THF are added. The mixture is refluxed for a further 40 min, cooled, a 1.25 M HCl solution in methanol is slowly added, the mixture is evaporated in a rotary evaporator. The residue is taken up in DCM, washed with a saturated sodium hydrogencarbonate solution. The organic phase is dried, filtered and evaporated. The brown oily residue is digested using a little ACN and filtered off with suction.

WORKUP

后处理

  1. temperatureto reflux
  2. temperatureThe mixture is refluxed for a further 40 min
  3. temperaturecooled
  4. customthe mixture is evaporated in a rotary evaporator
  5. washwashed with a saturated sodium hydrogencarbonate solution
  6. customThe organic phase is dried
  7. filtrationfiltered
  8. customevaporated
  9. filtrationfiltered off with suction