反应详情

温度

50 °C

10.59 g of O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyl-uronium hexafluorophosphate, 9.54 ml diisopropylethylamine and 1.26 g 1-hydroxy-7-azabenzotriazole are added to 4.50 g 3-benzyloxy-4-methyl-benzoic acid in 25 ml N,N-dimethylformamide under an argon atmosphere. The mixture is stirred for 15 minutes at ambient temperature, before 5.74 g N-(3-amino-5-tert-butyl-2-methoxyphenyl)methanesulphonamide-hydrochloride are added. The reaction mixture is stirred overnight at 50° C. After cooling to ambient temperature the reaction mixture is diluted with ethyl acetate, washed with water, 1 N hydrochloric acid and saturated aqueous sodium chloride solution, dried on magnesium sulphate and evaporated down. The flask residue is stirred with methanol, and the resulting white precipitate is suction filtered and dried.

1. additionare added
2. temperatureAfter cooling to ambient temperature the reaction mixture
3. washwashed with water, 1 N hydrochloric acid and saturated aqueous sodium chloride solution
4. customdried on magnesium sulphate
5. customevaporated down
6. stirringThe flask residue is stirred with methanol
7. filtrationfiltered
8. customdried