Trimethyl orthoformate → 1-Bromo-2-(dimethoxymethyl)-4,5-dimethoxybenzene

HRID 324033

反応式

HRID 324033 の反応式
[Br:1][C:2]1[C:7](C=O)=[CH:6][C:5]([O:10][CH3:11])=[C:4]([O:12][CH3:13])[CH:3]=1.[CH:14]([O:19][CH3:20])([O:17][CH3:18])OC>CO>[CH3:20][O:19][CH:14]([O:17][CH3:18])[C:7]1[C:2]([Br:1])=[CH:3][C:4]([O:12][CH3:13])=[C:5]([O:10][CH3:11])[CH:6]=1

参加物

4

反応物 2

HCID 9005Trimethyl orthoformateHCID 793516-Bromo-3,4-dimethoxybenzaldehyde

生成物 1

HCID 110771461-Bromo-2-(dimethoxymethyl)-4,5-dimethoxybenzene

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

6-Bromo-3,4-dimethoxybenzaldehyde (470 g) is suspended in methanol (600 ml), and thereto are added trimethyl orthoformate (1025 ml) and IRA-120 (H+-type, 10 g), and the mixture is refluxed for one hour. The mixture is cooled to room temperature, and the insoluble materials are removed by filtration, and the filtrate is concentrated under reduced pressure. The resulting residue is dissolved in ether, washed, dried, evaporated to remove the ether, and distilled under reduced pressure to give 6-bromo-3,4-dimethoxybenzaldehyde dimethyl acetal (522 g) as a main distillate (133-138° C./1 Torr).

後処理

  1. temperaturethe mixture is refluxed for one hour
  2. customthe insoluble materials are removed by filtration
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. dissolutionThe resulting residue is dissolved in ether
  5. washwashed
  6. customdried
  7. customevaporated
  8. customto remove the ether
  9. distillationdistilled under reduced pressure

出典と根拠

ORDレコード
ord-311d3a0a51d0408b98f9608191981361
出典データセット
uspto-grants-2001_04
特許番号
US06214996B1

関連ノート

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