HRID336142
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
Polymer-supported triphenylphosphine (˜3.0 mmol/g, 1.42 g) was added to a solution of 8-azido-5-(quinolin-3-yl)-6,7,8,9-tetrahydropyrimido[5,4-b]indolizin-4-amine (508 mg) obtained in Step 10 in THF (10 ml) and water (1 ml) at room temperature. The reaction mixture was heated under reflux for 1 hour. After cooling, the reaction mixture was filtered through Celite, washed with ethanol, and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (developing solvent: chloroform/methanol) to obtain the title compound as a yellow solid (342 mg). ESI-MS m/z 331 (MH+).
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureunder reflux for 1 hour
- temperatureAfter cooling
- filtrationthe reaction mixture was filtered through Celite
- washwashed with ethanol
- distillationthe solvent was distilled off under reduced pressure
- customThe resulting residue was purified by silica gel column chromatography (developing solvent: chloroform/methanol)