HRID49491

反应详情

EQUATION

反应方程式

HRID 49491 的结构方程式

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

  1. concentrationconcentrated
  2. dissolutiondissolved in water
  3. addition2M NaOH was added
  4. extractionthe inorganic phase was extracted with CH2Cl2
  5. washThe organic phase was washed with water
  6. dry with materialdried over Na2SO4
  7. customPurification by column chromatography with CH2Cl2/MeOH 20:1