反应详情

To a suspension of 3.3 g of the product of Example 3 in 50 ml of tetrahydrofuran was added dropwise 3 ml of condensed ammonia while keeping the reaction temperature at -5° C. with external cooling. After stirring at 0° for 1.5 hours, the solvent was evaporated in vacuo and water was added to the residue to yield a precipitate. After filtration the isolated residue was washed with water, then dissolved in tetrahydrofuran and dried over MgSO4. After evaporation of the solvent in vacuo, 2.9 g of the subject compound was obtained as a crude solid; m.p. 168°-173° C.

1. additionwas added dropwise
2. customat -5° C.
3. customthe solvent was evaporated in vacuo and water
4. additionwas added to the residue
5. customto yield a precipitate
6. filtrationAfter filtration the isolated residue
7. washwas washed with water
8. dissolutiondissolved in tetrahydrofuran
9. dry with materialdried over MgSO4
10. customAfter evaporation of the solvent in vacuo