反应详情

Under ice-cooling, 5.29 g (374 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was added to a solution of 8.84 g (23.0 mmol) of 4-[2-(4-methyl-1-piperazinyl)-4-thiazolyl]benzoic acid hydrobromide, 4.19 g (27.6 mmol) of 1-hydroxybenzotriazole, 6.44 g (27.6 mmol) of 1-aminocyclohexanecarboxylic acid phenylmethyl ester and 11.9 g (92 mmol) of N,N-diisopropylethylamine in 120 ml of dimethylformamide. After the mixture was stirred at room temperature overnight, under reduced pressure, the reaction solution was concentrated, ethyl acetate was added thereto, and the mixture was successively washed with water, a saturated aqueous sodium hydrogencarbonate solution and saturated brine, followed by drying with anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, ether was added to the residue and the crystal was washed to obtain 11.8 g (quantitative) of the title compound.

1. temperatureUnder ice-cooling
2. concentrationthe reaction solution was concentrated
3. additionethyl acetate was added
4. washthe mixture was successively washed with water
5. dry with materialby drying with anhydrous sodium sulfate
6. distillationAfter the solvent was distilled off under reduced pressure, ether
7. additionwas added to the residue
8. washthe crystal was washed