反应详情

A solution of 6-acetylamino-1-(3-methylbenzyl)-4-methyl-hexahydro-1H-1,4-diazepine (0.9 g) in 10% hydrochloric acid (20 ml) is refluxed with stirring for 2 hours. After cooling, the reaction mixture is basified with 48% aqueous sodium hydroxide solution and extracted with chloroform. The organic layer is washed with water and dried over magnesium sulfate. The solvent is evaporated under reduced pressure to give an oil. A mixture of this oil, 1H-indazole-3-carboxylic acid (530 mg), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (630 mg) and dichloromethane (20 ml) is stirred at 25° C. for 2 hours. The reaction mixture is washed successively with water and 10% aqueous sodium hydroxide solution, dried over magnesium sulfate, and evaporated under reduced pressure. The residue is chromatographed on silica gel with elution of acetone. Fractions containing the title compound are pooled and evaporated under reduced pressure to give the title compound (0.4 g) as an oil.

1. temperatureAfter cooling
2. extractionextracted with chloroform
3. washThe organic layer is washed with water
4. dry with materialdried over magnesium sulfate
5. customThe solvent is evaporated under reduced pressure
6. customto give an oil
7. stirringis stirred at 25° C. for 2 hours
8. washThe reaction mixture is washed successively with water and 10% aqueous sodium hydroxide solution
9. dry with materialdried over magnesium sulfate
10. customevaporated under reduced pressure
11. customThe residue is chromatographed on silica gel with elution of acetone
12. additionFractions containing the title compound
13. customevaporated under reduced pressure