反应详情

To a solution of the product of Example 3, Step b (0.85 g) and triethylamine (0.82 ml) at RT in dichloromethane (20 ml) was added methyl oxalyl chloride (0.30 ml) dropwise over 10 minutes. The reaction mixture was partitioned between water (20 ml) and dichloromethane (20 ml). The organic phase was separated and dried with MgSO4. Evaporation under reduced pressure gave an oil which was dissolved in ethanol (10 ml) at RT and treated with hydrazine hydrate (1 ml) The reaction mixture was stirred at reflux for 24 hours, filtered and the filtrate evaporated under reduced pressure to leave an oil. Purification by flash chromatography (dichloromethane:methanol 90:10)gave the sub-title compound as a white solid (0.18 g).

1. customThe reaction mixture was partitioned between water (20 ml) and dichloromethane (20 ml)
2. customThe organic phase was separated
3. dry with materialdried with MgSO4
4. customEvaporation under reduced pressure
5. customgave an oil which
6. temperatureat reflux for 24 hours
7. filtrationfiltered
8. customthe filtrate evaporated under reduced pressure
9. customto leave an oil
10. customPurification by flash chromatography (dichloromethane