反应详情

A solution of 60.1 mg (0.23 mmol) of the compound from example 1g in 1 ml of absolute DMF was mixed with 11 mg (0.23 mmol) of sodium hydride (50%) and stirred at RT for 1 h. Then 70.3 mg (0.23 mmol) of the compound from example 10a were added, and the mixture was stirred at RT for 1 h. The reaction solution was mixed with 1 ml of water and extracted several times with EA. The combined EA extracts were dried over Na2SO4, filtered and concentrated. Purification of the resulting residue by chromatography on silica gel with CH2Cl2/methanol (9:1) as mobile phase afforded 71.4 mg of the title compound.

1. stirringthe mixture was stirred at RT for 1 h
2. extractionextracted several times with EA
3. dry with materialThe combined EA extracts were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification of the resulting residue by chromatography on silica gel with CH2Cl2/methanol (9:1) as mobile phase