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Toluene → HCID 11745138, 화합물

HRID 256744
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HRID 256744 반응식
[Cl:1][C:2]([CH2:4]Cl)=[CH2:3].[C:6]1(=[O:12])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.C1(C)C=CC=CC=1>[Zn].C(O)(=O)C>[Cl:1][C:2](=[CH2:3])[CH2:4][C:6]1([OH:12])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1140TolueneHCID 65652,3-DichloropropeneHCID 7967Cyclohexanone

생성물 1

HCID 11745138HCID 11745138, 화합물수율 99%

시약·촉매·용매 2

HCID 23994Zinc촉매2회HCID 176Acetic Acid용매

실험 절차

56.53 Grams of 2,3-dichloro-1-propene were added dropwise to a mixture of 25.00 g of cyclohexanone, 75 g of toluene, 100 g of 5% acetic acid and 34.35 g of zinc powder at 45° C., and then the mixture was allowed to react at the same temperature for 3 hours. After the reaction was completed zinc-derived insolubles were filtered off, and the resultant filtrate was subjected to separation. The organic phase was washed with a 7% sodium carbonate aqueous solution and dried over sodium sulfate. The desiccant was filtered off, and then the toluene was distilled off under reduced pressure to give 44.05 g of 1-(2'-chloroallyl)-1-cyclohexanol. The results were as follows.

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후처리

  1. customto react at the same temperature for 3 hours
  2. filtrationwere filtered off
  3. customthe resultant filtrate was subjected to separation
  4. washThe organic phase was washed with a 7% sodium carbonate aqueous solution
  5. dry with materialdried over sodium sulfate
  6. filtrationThe desiccant was filtered off
  7. distillationthe toluene was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-865704b281e54e37a6856e16c5f5b572
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05258529

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