反应详情

温度

75 °C

trans-4-Amino-cyclohexanecarboxylic acid methyl ester hydrochloride (2 g, 10.3 mmol) was dissolved in a mixture of DMF (10 ml) and DIPEA (2 ml). Ethylformiate (5 ml, 62 mmol) were added and the mixture heated to 75° C. overnight. The solvent was evaporated and the crude product extracted from ethyl acetate. A brown oil was obtained. MS (ES+): 186 (M+H). The crude material was dissolved in dichloromethane (15 ml). Triethylamine (1.5 ml) was added and the reaction mixture cooled to 0° C. Triphosgene (470 mf, 1.6 mmol) was dissolved in dichloromethane (4 ml) and added drop wise to the reaction mixture. This was warmed up to rt and stirred for 1 h. The product was isolated directly via Kieselgel chromatography using ethyl acetate as an eluent. The intermediate was used without further characterization.

1. additionEthylformiate (5 ml, 62 mmol) were added
2. customThe solvent was evaporated
3. extractionthe crude product extracted from ethyl acetate
4. customA brown oil was obtained
5. temperaturethe reaction mixture cooled to 0° C
6. additionadded drop wise to the reaction mixture
7. temperatureThis was warmed up to rt
8. customThe product was isolated directly via Kieselgel chromatography