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

HRID 34292

反応式

HRID 34292 の反応式
[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]

参加物

6

反応物 3

HCID 24408Bromine2 回HCID 2303074-Iodo-1,2-dimethoxybenzeneHCID 23665763Sodium Bisulfite

生成物 1

HCID 33464041-Bromo-2-iodo-4,5-dimethoxybenzene収率 95%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-611285cd275a424f86977e849e6ea951
出典データセット
uspto-grants-1988_08
特許番号
US04761413

関連ノート

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