1,2-Dichloroethane → HCID 22404520, 화합물

HRID 256732노트

반응식

HRID 256732 반응식
[Cl:1][C:2](CCl)=[CH2:3].[C:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])[CH3:7].[CH2:15](Cl)CCl>[Zn].C(O)(=O)C>[Cl:1][C:2]([CH2:7][C:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([OH:8])[CH3:15])=[CH2:3]

참가 물질

6

반응물 3

HCID 111,2-DichloroethaneHCID 65652,3-DichloropropeneHCID 7410Acetophenone

생성물 1

HCID 22404520HCID 22404520, 화합물

시약·촉매·용매 2

HCID 23994Zinc촉매2회HCID 176Acetic Acid용매

실험 절차

33.26 of 2,3-dichloro-1-propene were added dropwise to a mixture of 20.00 g of acetophenone, 40 g of ethylene dichloride, 60 g of 5% acetic acid and 19.52 g of zinc powder at 50° C., and the resultant mixture was allowed to react at the same temperature for 10 hours. After the reaction was completed, zinc-derived insolubles were filtered off, and the resultant 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 ethylene dichloride was distilled off under reduced pressure. The resultant oily substance was purified by silica gel column chromatography to give 22.24 g of 2-chloro-4-phenyl-1-penten-4-ol; nD25 =1.536, FI-MS m/e 178(M-H2O+), 180 (M-H2O+2+).

후처리

  1. customto react at the same temperature for 10 hours
  2. filtrationwere filtered off
  3. customthe resultant filtrate was separated
  4. washThe organic phase was washed with 7% sodium carbonate aqueous solution
  5. dry with materialdried over magnesium sulfate
  6. filtrationThe desiccant was filtered off
  7. distillationthe ethylene dichloride was distilled off under reduced pressure
  8. customThe resultant oily substance was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-3a158cd03a984df6a1405ea3e91eab19
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258529

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