HRID1777737
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
To an ice-cold solution of methyl 1H-pyrrolo[2,3-b]pyridine-2-carboxylate (300 mg) in THF (4.5 mL) was added LiAlH4 (1.7 mL, 1M in THF). The ice bath was removed and the reaction mixture was stirred at RT for 2 h. LiAlH4 (2.8 mL, 1M in THF) was added and the stirring was pursued for 20 h at RT. DCM and 1M NaOH were added and the phases were separated. The org. layer was dried (Na2SO4) and evaporated in vacuo to afford 100 mg of oil. LC-MS (B): tR=0.34 min; [M+H]+: 149.28.
WORKUP
后处理
- customThe ice bath was removed
- additionLiAlH4 (2.8 mL, 1M in THF) was added
- waitthe stirring was pursued for 20 h at RT
- additionDCM and 1M NaOH were added
- customthe phases were separated
- dry with materiallayer was dried (Na2SO4)
- customevaporated in vacuo