反应详情

23 ml of a 15% solution of TiCl3 was added to 1.6 g of N-(β-methoxy-ethyl)-N-[4-phenoxy-(4'-nitro)-benzyl]-dichloroacetamide, in 30 ml of acetone; the pH was then adjusted to 3 with 23% HCl. The resulting mixture was stirred at room temperature for 24 hours and then, with cooling, brought to pH 9 with concentrated ammonium hydroxide. The resulting precipitate was removed by filtration and washed with water. The filtrated was extracted several times with chloroform. The combined organic extract was then dried on Na2SO4 and evaporated to dryness to give 1.2 g of N-(β-methoxy-ethyl)-N-[4-phenoxy-(4'-amino)-benzyl]-dichloroacetamide, m.p. 100°-102° C.

1. temperaturewith cooling
2. customThe resulting precipitate was removed by filtration
3. washwashed with water
4. extractionThe filtrated was extracted several times with chloroform
5. extractionThe combined organic extract
6. customwas then dried on Na2SO4
7. customevaporated to dryness