HRID968490
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
A solution of intermediate (8) (0.072 mol) and BTEAC (0.0362 mol) in ACN (150 ml) was stirred at room temperature. Phosphoric trichloride (0.222 mol) was added dropwise. The mixture was stirred and refluxed for 8 hours. The solvent was evaporated till dryness. The residue was poured out into water and NH4OH. The mixture was extracted with DCM. The organic layer was separated, dried, filtered and the solvent was evaporated, yielding 15 g of 2-chloro-5,6,7,8-tetrahydro-3-nitroquinoline (intermediate 9).
WORKUP
后处理
- temperaturerefluxed for 8 hours
- customThe solvent was evaporated till dryness
- additionThe residue was poured out into water and NH4OH
- extractionThe mixture was extracted with DCM
- customThe organic layer was separated
- customdried
- filtrationfiltered
- customthe solvent was evaporated