反应详情

温度

0 °C

To a THF (5 ml) solution of the compound of Example 41 B (1.4 g, 5.5 mmol) and (R)-(+)-2-methyl-2-propanesulfinylamide (1.0 g, 8.26 mmol), titanium(IV) ethoxide (5.0 ml, 21.9 mmol) was added under a nitrogen atmosphere and the mixture was subjected to microwave irradiation at at 70° C. with stirring for 2.5 hours. After imine formation was confirmed with LC-MS (MS (ESI) m/z 347 (M−H)−, 349 (M+H)+), the mixture was cooled to 0° C. and sodium borohydride (707 mg, 18.7 mmol) was added and the reaction mixture was stirred for 2 hours at 0° C. The reaction mixture was partitioned with water and ethanol, then the mixture was stirred for 1 hour at room temperature. The mixture was filtrated through a Celite pad, and the filtrate was evaporated and concentrated in vacuo to give the title compound (1.9 g, 99%).

1. customirradiation at at 70° C.
2. stirringthe reaction mixture was stirred for 2 hours at 0° C
3. customThe reaction mixture was partitioned with water and ethanol
4. stirringthe mixture was stirred for 1 hour at room temperature
5. filtrationThe mixture was filtrated through a Celite pad
6. customthe filtrate was evaporated
7. concentrationconcentrated in vacuo