反应详情

1-Hydroxybenzotriazole (273 mg, 2.0 mmol), 3-phenylpropylamine (0.142 ml, 1.0 mmol) and N-methylmorpholine (0.222 ml, 2.0 mmol) were added to a solution of (4-dimethylamino-4-phenylcyclohexyl)acetic acid hydrochloride (298 mg, 1.0 mmol) in dry dimethylformamide under argon. Dicyclohexylcarbodiimide (417 mg, 2.0 mmol) was added to the clear solution at 0° C. The reaction mixture was stirred at RT for 3 d, the urea which had precipitated out was filtered off with suction and the filtrate was introduced into a mixture of saturated NaCl solution (40 ml) and saturated NaHCO3 solution (10 ml). 5 M sodium hydroxide solution (12 ml, 60 mmol) was added to the aqueous phase and the mixture was diluted with water (300 ml) and stored at 5° C. for 3 d. The product was thereby produced as a colourless compound and was to be obtained in a yield of 58% (220 mg) by filtration, taking up of the residue in ethanol and concentration.

1. customthe urea which had precipitated out
2. filtrationwas filtered off with suction
3. additionthe filtrate was introduced into a mixture of saturated NaCl solution (40 ml) and saturated NaHCO3 solution (10 ml)
4. waitstored at 5° C. for 3 d
5. customThe product was thereby produced as a colourless compound
6. customto be obtained in a yield of 58% (220 mg) by filtration
7. concentrationconcentration