Bromine → 1-Bromo-2-iodo-4,5-dimethoxybenzene

HRID 1165466

반응식

HRID 1165466 반응식
[I:1][C:2]1[CH:3]=[C:4]([O:10][CH3:11])[C:5]([O:8][CH3:9])=[CH:6][CH:7]=1.[Br:12]Br.S(=O)(O)[O-].[Na+]>C(O)(=O)C.O>[Br:12][C:7]1[CH:6]=[C:5]([O:8][CH3:9])[C:4]([O:10][CH3:11])=[CH:3][C:2]=1[I:1]

참가 물질

6

반응물 3

HCID 24408Bromine2회HCID 2303074-Iodo-1,2-dimethoxybenzeneHCID 23665763Sodium Bisulfite

생성물 1

HCID 33464041-Bromo-2-iodo-4,5-dimethoxybenzene수율 95%

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 962Water용매

실험 절차

4-Iodoveratrole (26.0 g, 0.0985M) in acetic acid (25 ml) was treated with bromine (6.5 ml, 0.127M) in acetic acid (30 ml) and stirred at room temperature for one hour. The mixture was diluted with water (300 ml) and treated with sodium bisulfite to discharge the excess bromine. The white solid was filtered, washed with water and dried in vacuo over P2O5 to give 4-bromo-5-iodoveratrole (33.0 g, 95% yield) as a white solid, mp 98°-100° C. (literature: Baker et al., J. Chem. Soc. 3986 (1961), mp 102°-104° C.). NMR (CDCl3) δ 3.83 ppm (s, 6H, (2x) OCH3), 7.06 (s, 1H, ArH), 7.21 (s, 1H, ArH).

후처리

  1. filtrationThe white solid was filtered
  2. washwashed with water
  3. dry with materialdried in vacuo over P2O5

출처 및 근거

ORD 기록
ord-ec6178f1dbfa4a42b8c30e2230e03b8e
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04910198

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