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

HRID 444075노트

반응식

HRID 444075 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 23925Iron촉매HCID 5943Carbon Tetrachloride용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e80750713554475f8b42d2bf142d562b
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04263037

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