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
Under an argon atmosphere 361 mg (1.88 mmol) of dimethyl (1-diazo-2-oxopropyl)phosphonate in 4 mL of MeOH was added to a solution of 300 mg (1.57 mmol) of 3-(6-isopropylaminopyridin-3-yl)propionaldehyde and 434 mg (3.14 mmol) of potassium carbonate in 6 mL of MeOH and the mixture was stirred for 3 hours at RT. The reaction mixture was diluted with water and EtOAc, combined with saturated aqueous sodium hydrogen carbonate solution, and the organic phase was separated off, extracted with water, dried over magnesium sulfate, filtered, and the solvent was removed in vacuo. Yield: 220 mg (75% of theoretical); C12H16N2 (M=188.269); calc.: molpeak (M+H)+:189; found: molpeak (M+H)+:189; HPLC-MS: 4.09 minutes (method G).
WORKUP
后处理
- customthe organic phase was separated off
- extractionextracted with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customthe solvent was removed in vacuo
- custom4.09 minutes (method G)