反应详情

A mixture of 1.4 g of ferric nitrate in 1200 ml of liquid ammonia was formed at -60° C. and was then stirred for 5 minutes after which 2 g of sodium were added thereto at -60° C. The mixture was stirred for 10 minutes and 104 g of sodium were added at -55°±5° C. over 21/2 hours. The mixture was stirred at -55° C. for one hour. 300 g of ethyl acetylacetate were added thereto over 30 minutes at less than -30° C. 1000 ml of ether at -20° C. were added to the mixture which was then stirred for 5 minutes. 289 g of 1-chloro-3-methyl-2-butene were added over 30 minutes at less than -25° C. and the mixture stood at room temperature for 17 hours. 1000 ml of ether were progressively added at less than +15° C. followed by a solution of 250 ml of acetic acid in 1000 ml of water. The decanted aqueous phase was extracted with ether and the combined organic phases were washed with 2 N hydrochloric acid, then with water, dried over sodium sulfate and evaporated to dryness under reduced pressure. The residue was rectified under reduced pressure to obtain 175.5 g of ethyl 7-methyl-3-oxo-6-octenoate with a boiling point of 98° to 107° C. at 3 mm Hg.

1. customwas formed at -60° C.
2. additionwere added
3. customat -60° C
4. stirringThe mixture was stirred at -55° C. for one hour
5. waitover 30 minutes at less than -30° C
6. stirringwas then stirred for 5 minutes
7. waitthe mixture stood at room temperature for 17 hours
8. extractionThe decanted aqueous phase was extracted with ether
9. washthe combined organic phases were washed with 2 N hydrochloric acid
10. dry with materialwith water, dried over sodium sulfate
11. customevaporated to dryness under reduced pressure