反应详情

24 g of iron powder was added to a solution of 1.6 ml of concentrated HCl, 16.8 ml of water, and 70 ml of ethanol. 29.6 g of the 2-chloro-5-nitrobenzoyl acetate prepared above in Step 2 dissolved in 45 ml of ethanol, was then added to the mixture in three equal portions. The resultant reaction mixture was refluxed for 5 hours. An additional 2.4 g of iron and 0.1 ml of concentrated HCl was then added to the reaction mixture. The reaction mixture was then refluxed for an additional one hour, filtered through Celite and evaporated. 100 ml of water was then added to the evaporated material and the resultant mixture was extracted with 100 ml of ether. The ether solution was washed with water, dried over magnesium sulfate, and evaporated, to produce 22.9 g of 5-amino-2-chlorobenzoyl acetate as an oil.

1. additionwas then added to the mixture in three equal portions
2. customThe resultant reaction mixture
3. temperaturewas refluxed for 5 hours
4. temperatureThe reaction mixture was then refluxed for an additional one hour
5. filtrationfiltered through Celite
6. customevaporated
7. addition100 ml of water was then added to the evaporated material
8. extractionthe resultant mixture was extracted with 100 ml of ether
9. washThe ether solution was washed with water
10. dry with materialdried over magnesium sulfate
11. customevaporated