反应详情

To a solution of Intermediate 1 (0.5 g, 3.57 mmol) in a mixture of 1,4-dioxane (4 mL) and N,N-dimethylformamide (1 mL), cyclopropanecarbonyl chloride (ALDRICH, 0.49 mL, 5.35 mmol) was added and the resulting mixture was heated under reflux overnight. The reaction was then concentrated under vacuum yielding a pale yellow solid which was purified by flash chromatography (Si, eluting with DCM:MeOH mixtures, gradient from 100:0% to 90:10%) to yield a beige solid which was re-purified by flash chromatography (Si, eluting with DCM:MeOH mixtures from 100:0 to 85:15%). The title compound was obtained as a white solid.

1. additionwas added
2. temperaturethe resulting mixture was heated
3. temperatureunder reflux overnight
4. concentrationThe reaction was then concentrated under vacuum
5. customyielding a pale yellow solid which
6. customwas purified by flash chromatography (Si, eluting with DCM:MeOH mixtures, gradient from 100:0% to 90:10%)
7. customto yield a beige solid which
8. customwas re-purified by flash chromatography (Si, eluting with DCM:MeOH mixtures from 100:0 to 85:15%)