HRID49491
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
To 560 mg (1.4 mmol) 6-(5-Methanesulfonyloxy-pentyl)-3,4-dihydro-2H-quinoline-1-carboxylic acid tert-butyl ester in 5 ml DMF were added 2.5 ml (26.0 mmol) N-allylmethylamine. The solution was stirred at 70° C. for 2 h, concentrated and dissolved in water and CH2Cl2. 2M NaOH was added and the inorganic phase was extracted with CH2Cl2. The organic phase was washed with water and dried over Na2SO4. Purification by column chromatography with CH2Cl2/MeOH 20:1 yielded 470 mg (89%) 6-[5-(Allyl-methyl-amino)-pentyl]-3,4-dihydro-2H-quinoline-1-carboxylic acid tert-butyl ester as yellow oil, MS: 373 (MH+).
WORKUP
后处理
- concentrationconcentrated
- dissolutiondissolved in water
- addition2M NaOH was added
- extractionthe inorganic phase was extracted with CH2Cl2
- washThe organic phase was washed with water
- dry with materialdried over Na2SO4
- customPurification by column chromatography with CH2Cl2/MeOH 20:1