HRID1963264
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
Methyl 4-((tert-butyldimethylsilyloxy)methyl)-2-(3,3-dimethylbutyl)piperidine-1-carboxylate (3.606 g, 9.7 mmol) was dissolved in THF (50 mL) and TBAF (1M in THF) (13 mL, 13 mmol) added. Stirred at room temperature for 3.5 h. The solvent was evaporated. Redissolved in DCM and washed with satd NaHCO3. The organic phase was passed through a phase separator and evaporated to yield an oil. The residue was purified via Biotage (eluent 30-70% EtOAc in heptane) to yield methyl 2-(3,3-dimethylbutyl)-4-(hydroxymethyl)piperidine-1-carboxylate (2.45 g, 98%) as a colourless oil. MS m/z 258 (M+H)+
WORKUP
后处理
- customThe solvent was evaporated
- dissolutionRedissolved in DCM
- washwashed with satd NaHCO3
- customevaporated
- customto yield an oil
- customThe residue was purified via Biotage (eluent 30-70% EtOAc in heptane)