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
The compound (203.5 mg) obtained in Example 9-2 was dissolved in anhydrous methanol (8.1 ml) and added with 6,7-dihydro-5H-quinolin-8-one (117.7 mg) which was synthesized by a known method and sodium cyanoborohydride (99.9 mg). After the solution was adjusted to pH 5 with acetic acid, the whole was stirred at room temperature for 2 days. After completion of the reaction, the solvent was distilled off. The resultant was added with a 1 mol/l sodium hydroxide aqueous solution and the whole was subjected to extraction with chloroform. The resultant was dried with magnesium sulfate and the solvent was distilled off. The residue was purified through silica gel column chromatography (chloroform/ethyl acetate) and treated with hydrochloric acid, thereby obtaining a hydrochloride (69.5 mg) of the subject compound as a pale-yellow solid.
WORKUP
后处理
- customAfter completion of the reaction
- distillationthe solvent was distilled off
- additionThe resultant was added with a 1 mol/l sodium hydroxide aqueous solution
- extractionthe whole was subjected to extraction with chloroform
- dry with materialThe resultant was dried with magnesium sulfate
- distillationthe solvent was distilled off
- customThe residue was purified through silica gel column chromatography (chloroform/ethyl acetate)
- additiontreated with hydrochloric acid