Iodine → 5-Bromo-3,3-dimethylbenzofuran-2(3H)-one

HRID 1155949

反応式

HRID 1155949 の反応式
[CH3:1][C:2]1([CH3:12])[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][C:3]1=[O:11].II.[Br:15]Br>C(Cl)(Cl)(Cl)Cl.[Fe]>[Br:15][C:8]1[CH:9]=[CH:10][C:5]2[O:4][C:3](=[O:11])[C:2]([CH3:12])([CH3:1])[C:6]=2[CH:7]=1

参加物

6

反応物 3

HCID 807IodineHCID 24408BromineHCID 5956202(3H)-Benzofuranone, 3,3-dimethyl-

生成物 1

HCID 162206345-Bromo-3,3-dimethylbenzofuran-2(3H)-one

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 5943Carbon Tetrachloride溶媒

実験手順

2,3-Dihydro-3,3-dimethylbenzofuran-2-one (1.62 g, 0.01 mole), in carbon tetrachloride (25 ml) containing catalytic amounts of iron filings and iodine was treated with bromine (1.6 g, 0.01 mole) and the mixture boiled under reflux for 1 hour. The solvent was removed under vacuum and the residue taken up in petroleum ether (b.p. 60°-80° C.). The solution was decanted from a little insoluble residue and washed with aqueous sodium metabisulphite and water, dried over magnesium sulphate and run down. The title product was obtained as a white solid m.p. 49°-53° C. and was shown by NMR to be a slightly impure sample of the product obtained in Example 3(b).

後処理

  1. temperatureunder reflux for 1 hour
  2. customThe solvent was removed under vacuum
  3. customThe solution was decanted from a little insoluble residue
  4. washwashed with aqueous sodium metabisulphite and water
  5. dry with materialdried over magnesium sulphate

出典と根拠

ORDレコード
ord-08b44c19d50a487ba35eaa88d01d0b12
出典データセット
uspto-grants-1982_06
特許番号
US04333759

関連ノート

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