Chloroform → 1-(2-Bromoethenyl)-4-methoxynaphthalene

HRID 1287928노트

반응식

HRID 1287928 반응식
C([CH:4]=[CH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([O:16][CH3:17])=[CH:8][CH:7]=1)(O)=O.C(Cl)(Cl)Cl.[Br:22]Br.C(=O)([O-])[O-].[Na+].[Na+]>O.C(Cl)Cl>[Br:22][CH:4]=[CH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([O:16][CH3:17])=[CH:8][CH:7]=1

참가 물질

7

반응물 4

HCID 6212ChloroformHCID 10340Sodium CarbonateHCID 24408BromineHCID 38801493-(4-methoxynaphthyl)acrylic acid

생성물 1

HCID 544133521-(2-Bromoethenyl)-4-methoxynaphthalene

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a suspension of 33.3 g. (0.146 mol.) of 1-(2-carboxyethenyl)-4-methoxynaphthalene in 500 ml. of chloroform was added dropwise a solution of 8.05 ml. (0.146 mol.) of bromine in 125 ml. of methylene chloride. The solvent was removed, a solution of 31 g. (0.292 mol.) of sodium carbonate in 300 ml. of water was added to the residue and the mixture was refluxed for 2 hours. After cooling, the mixture was extracted with methylene chloride, the layers were separated and the organic phase was washed with water and saturated sodium chloride solution, dried (MgSO4) and evaporated to dryness to give 1-(2-bromoethenyl)-4-methoxynaphthalene.

후처리

  1. additionTo a suspension of 33.3 g
  2. customThe solvent was removed
  3. temperaturethe mixture was refluxed for 2 hours
  4. temperatureAfter cooling
  5. extractionthe mixture was extracted with methylene chloride
  6. customthe layers were separated
  7. washthe organic phase was washed with water and saturated sodium chloride solution
  8. dry with materialdried (MgSO4)
  9. customevaporated to dryness

출처 및 근거

ORD 기록
ord-6f2f20a1e221434ab754b98afa291f7a
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03985896

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