HRID2262846
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of (±)-2-hydroxy-6,8-dihydrospiro[cyclopenta[g]quinoline-7,3′-pyrrolo[2,3-b]pyridin]-2′(1′H)-one from Step B (3.00 g, 9.89 mmol) in POCl3 (30 mL) was stirred at 80° C. for 2 h, then concentrated to dryness under reduced pressure. The residue was partitioned between saturated aqueous NaHCO3 (200 mL) and CH2Cl2 (500 mL). The aqueous layer was extracted further with CH2Cl2 (200 mL). The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure to give the title compound. MS: m/z=322 (M+1).
WORKUP
后处理
- concentrationconcentrated to dryness under reduced pressure
- customThe residue was partitioned between saturated aqueous NaHCO3 (200 mL) and CH2Cl2 (500 mL)
- extractionThe aqueous layer was extracted further with CH2Cl2 (200 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure