反应详情

温度

85 °C

1-(5-Iodo-pyridin-2-yl)-cyclobutane carboxylic acid (3.92 g, 12.9 mmol) was combined with tert-BuOH (6.1 mL, 65 mmol), Et3N (9.0 mL, 65 mmol) and DPPA (3.1 mL, 14 mmol). The reaction was heated to reflux (external bath: 85° C.) for 1.5 h. The volatiles were removed in vacuo and the crude reaction mixture was purified by normal phase flash chromatography on silica gel (5→80% EtOAc/hexanes) to give 1.1 g of [1-(5-iodo-pyridin-2-yl)-cyclobutyl]-carbamic acid tert-butyl ester as a solid, m/z 375.4 [M+H]+.

1. temperatureThe reaction was heated
2. customThe volatiles were removed in vacuo
3. customthe crude reaction mixture
4. customwas purified by normal phase flash chromatography on silica gel (5→80% EtOAc/hexanes)