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1-Bromo-3-chloropropane → 1-[4-(3-Chloropropoxy)-3-methylphenyl]ethanone

HRID 1193649
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반응식

HRID 1193649 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]([CH3:10])=[O:9])[CH:5]=[CH:4][C:3]=1[OH:11].Br[CH2:13][CH2:14][CH2:15][Cl:16].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:16][CH2:15][CH2:14][CH2:13][O:11][C:3]1[CH:4]=[CH:5][C:6]([C:8](=[O:9])[CH3:10])=[CH:7][C:2]=1[CH3:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 701354'-Hydroxy-3'-methylacetophenone

생성물 1

HCID 144071751-[4-(3-Chloropropoxy)-3-methylphenyl]ethanone수율 95.1%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 25 g (0.166 mole) of 4-hydroxy-3-methylacetophenone, 45.8 g (0.33 mole) of 1-bromo-3-chloropropane and 69.1 g (0.5 mole) of anhydrous potassium carbonate in 500 ml of acetone was heated at reflux for 20 hr. The mixture was cooled, filtered, and the filtrate concentrated under reduced pressure to give an oil as residue. The oil was crystallized in petroluem ether. The solid was collected by filtration, washed with petroleum ether and dried to yield 35.8 g (95%) of an off-white powder. An analytical sample, m.p. 41.5°-42.5° C. was prepared from petroleum ether.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 20 hr
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated under reduced pressure
  6. customto give an oil as residue
  7. customThe oil was crystallized in petroluem ether
  8. filtrationThe solid was collected by filtration
  9. washwashed with petroleum ether
  10. customdried

출처 및 근거

ORD 기록
ord-829dc3e901ef4d2dac2b82cc6015a0ee
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04810713

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