反应详情

To a solution of 4-hydrazino-2-methyl-6-phenylpyrimidine trihydrochloride (300 mg, 0.97 mmol) and diisopropylethylamine (0.17 mL, 0.97 mmol) in ethanol (10 mL) was added 4-dimethylaminoacetophenone (158 mg, 0.97 mmol). The resultant reaction mixture was heated at reflux overnight. The reaction mixture was diluted with dIH2O and the pH was adjusted to 1-2 and washed with ethyl acetate. The pH of the aqueous layer was adjusted to 9-10 and was extracted with ethyl acetate. The combined extracts were concentrated in vacuo and the residue crystallized from ethyl acetate:hexanes. 60 mg (18%) of the title compound was isolated as a yellow solid. HPLC Purity: 98%.

1. customThe resultant reaction mixture
2. temperaturewas heated
3. temperatureat reflux overnight
4. additionThe reaction mixture was diluted with dIH2O
5. washwashed with ethyl acetate
6. extractionwas extracted with ethyl acetate
7. concentrationThe combined extracts were concentrated in vacuo
8. customthe residue crystallized from ethyl acetate