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

HRID 324033

반응식

HRID 324033 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-311d3a0a51d0408b98f9608191981361
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06214996B1

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