反应详情

A solution of 90% (fuming) nitric acid (22 ml) and glacial acetic acid (11 ml) cooled at 12° C. was treated in portions with solid compound from Example 3B (5.4 g, 27.7 mmoles) so as to maintain the temperature of <17° C. After the addition, stirring was continued for 15 minutes, when the internal temperature began to fall. The mixture was diluted to 100 ml with water, the yellow solid filtered, washed with water, taken up in CH2Cl2, dried (Na2SO4) and evaporated to give 5.43 g (82%) of pure title compound.

1. temperatureto maintain the temperature of <17° C
2. additionAfter the addition
3. filtrationthe yellow solid filtered
4. washwashed with water
5. dry with materialdried (Na2SO4)
6. customevaporated