反应详情

An aqueous methylamine solution (5 mL, 40%, 58.7 mmole) was mixed with XII (200 mg, 0.08 mmole) and stirred for 3 hr. in a sealed tube at 45° C. After the reaction was complete, water (10 mL) was added to the cooled reaction mixture, and the reaction mixture was extracted with chloroform (10×5 mL). The combined organic extracts were dried over anhydrous sodium sulfate, filtered and concentrated. The residue obtained was chromatographed on a silica gel column using methanol:chloroform (1:9) and then with a chloroform: methanol mixture containing 1% triethylamine as eluent. About 70 mg of XIII was obtained as a slightly yellow syrup, which was distilled at 110°-112° C., 0.04 mm Hg. XIII was converted to its mono fumarate salt form, which exhibits a melting point of 103°-104° C.

1. customat 45° C
2. extractionthe reaction mixture was extracted with chloroform (10×5 mL)
3. dry with materialThe combined organic extracts were dried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue obtained
7. customwas chromatographed on a silica gel column
8. additionwith a chloroform: methanol mixture containing 1% triethylamine as eluent