HRID1401864
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto reflux
- temperatureThe mixture is refluxed for a further 40 min
- temperaturecooled
- customthe mixture is evaporated in a rotary evaporator
- washwashed with a saturated sodium hydrogencarbonate solution
- customThe organic phase is dried
- filtrationfiltered
- customevaporated
- filtrationfiltered off with suction