반응 #343912

반응 방정식

2,3-dichloro-1-propene

methyl 2-methyl-1-propenyl ketone

toluene

→

2-chloro-4,6-dimethyl-1,5-heptadien-4-ol

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONafter the addition
2. 2
   여과were filtered off
3. 3
   기타the filtrate was separated
4. 4
   세척The organic phase was washed with 7% sodium carbonate aqueous solution
5. 5
   건조dried over magnesium sulfate
6. 6
   여과The desiccant was filtered off
7. 7
   workup.DISTILLATIONthe toluene was distilled off under reduced pressure
8. 8
   기타The resultant oily substance was purified by silica gel column chromatography

실험 절차

45.23 Grams of 2,3-dichloro-1-propene were added dropwise to a mixture of 20.00 g of methyl 2-methyl-1-propenyl ketone, 60 g of toluene, 60 g of water and 26.65 g of zinc powder at 35° C., and after the addition, the resultant mixture was maintained at the same temperature for 5 hours. After the reaction was completed zinc-derived insolubles were filtered off, and the filtrate was separated. The organic phase was washed with 7% sodium carbonate aqueous solution and dried over magnesium sulfate. The desiccant was filtered off and the toluene was distilled off under reduced pressure. The resultant oily substance was purified by silica gel column chromatography to give 31.11 g of 2-chloro-4,6-dimethyl-1,5-heptadien-4-ol; nD25 =1.474, FI-MS m/e 174(M), 176(M+2).

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