反应详情

A suspension of acetaldehyde N1 -(7-chloroquinazolin-4-yl)-p-methoxyphenylhydrazone hydrochloride (15.0g.) in ethanol (120ml.; dried over magnesium ethoxide) was cooled and stirred at 5°-10° C for 3 hrs. during the passage of dry hydrogen chloride. The mixture was then left at 0°-5° C. for 3 days before separation by filtration. The solid was washed with dry ether (10ml.), and then dissolved in a mixture of water (30ml.), saturated sodium acetate solution (5ml.) and ethyl acetate (25ml.). The aqueous layer was extracted with more ethyl acetate (2 × 15ml.), and the extracts washed with water (20ml.), dried (Na2SO4) and evaporated to give N1 -(7-chloroquinazolin-4-yl)-p-methoxyphenylhydrazine, m.p. 124°-127° C.

1. temperaturewas cooled
2. waitThe mixture was then left at 0°-5° C. for 3 days before separation by filtration
3. washThe solid was washed with dry ether (10ml.)
4. dissolutiondissolved in a mixture of water (30ml.), saturated sodium acetate solution (5ml.) and ethyl acetate (25ml.)
5. extractionThe aqueous layer was extracted with more ethyl acetate (2 × 15ml.)
6. washthe extracts washed with water (20ml.)
7. dry with materialdried (Na2SO4)
8. customevaporated