反应详情

To glacial HOAc (860 mL) was added red fuming HNO3 (300 mL) with cooling and stirring, at such a rate that the temperature was kept below 20° C. This stirred mixture was cooled in an ice bath and the foregoing material prepared in Example 134 (200 g, 78% pure, 1.1 mol) was added in portions over a period of 1 hr such that the temperature was maintained between 18°-20° C. The reaction was then stirred overnight. The precipitate which formed was filtered off and washed with HOAc (50 mL). This solid was then slurried with ice-H2O (400 mL), filtered off and dried to constant weight in vacuo at 60° C. to yield 141 g (0.75 mol, 68% yield) of the title compound; nmr (d6 -DMSO) d: 3.95 (s); mass spectrum showed m/e 187 (M+). A separate synthesis gave an analytical sample.

1. temperaturewith cooling
2. customwas kept below 20° C
3. temperatureThis stirred mixture was cooled in an ice bath
4. temperaturewas maintained between 18°-20° C
5. stirringThe reaction was then stirred overnight
6. customThe precipitate which formed
7. filtrationwas filtered off
8. washwashed with HOAc (50 mL)
9. filtrationfiltered off
10. customdried to constant weight in vacuo at 60° C.