反应详情

Subsequently, under ice-cooled condition, to 9.3 g (37 mmol) of phenylmethyl (2RS,3S)-3-amino-2-hydroxyheptanoate, 9.5 g (37 mmol) of 1-[N-(morpholine-4-carbonyl)amino]cyclohexanecarboxylic acid synthesized in Reference Example 5 and 6.0 g (45 mmol) of 1-hydroxybenzotriazole in 100 ml of dichloromethane, 8.5 g (45 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was added and then was stirred at the room temperature for 18 hours. The reaction solution was concentrated under reduced pressure. The residue was washed successively with water, aqueous solution of 10% of potassium hydrogensulfate, aqueous solution of saturated sodium hydrogen-carbonate and saturated brine in addition of ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and the solvent was distilled away from the reaction mixture under reduced pressure. The residue was purified by the silicagel column chromatography, whereby 16.8 g of phenylmethyl (2RS,3S)-2-hydroxy-3-[N-[1-[N-(morpholine-4-carbonyl)amino]cyclohexanecarbonyl]amino]heptanoate was obtained.

1. temperatureSubsequently, under ice-cooled condition
2. additionwas added
3. concentrationThe reaction solution was concentrated under reduced pressure
4. washThe residue was washed successively with water, aqueous solution of 10% of potassium hydrogensulfate, aqueous solution of saturated sodium hydrogen-carbonate and saturated brine in addition of ethyl acetate
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. distillationthe solvent was distilled away from the reaction mixture under reduced pressure
7. customThe residue was purified by the silicagel column chromatography