反应详情

A solution of 450 mg (1.25 mmol) of the end product of Example 25 in 10 ml of acetic acid and 1 ml of 30% hydrogen peroxide was allowed to stand at room temperature overnight. The solution was treated with ice and ammonium hydroxide; the resulting solid was collected, washed with water, dissolved in methylene chloride, treated with anhydrous sodium sulfate and charcoal, filtered and evaporated in vacuo to a white foam, mp 95°-110°: Ir (KBr) 1610, 1480 and 1047 cm-1 ; nmr (CDCl3) 2.95 (s, 3H), 4.15 (d, J=13 Hz, 1H), 5.25 (d, J=13 Hz, 1H), 6.95-8.40 (m, aromatic, 8H); uv λ max 219 nm (ε=37500), infl. 243 (20000); sh. 265 (13700), infl. 305 (1200); mass spectrum m/e 373 (M+).

1. customthe resulting solid was collected
2. washwashed with water
3. dissolutiondissolved in methylene chloride
4. additiontreated with anhydrous sodium sulfate and charcoal
5. filtrationfiltered
6. customevaporated in vacuo to a white foam, mp 95°-110°