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

HRID 1287928ノート

反応式

HRID 1287928 の反応式
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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6f2f20a1e221434ab754b98afa291f7a
出典データセット
uspto-grants-1976_10
特許番号
US03985896

反応ノート

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