Hydrogen Bromide →

HRID 1060578

반응식

HRID 1060578 반응식
[CH:1]([C:3]1[CH:11]=[C:10]([O:12][CH3:13])[C:9]([O:14][CH3:15])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6])=O.[C:16]1([P:22]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.Br>C(O)(=O)C.C(#N)C.C(OCC)C>[CH3:13][O:12][C:10]1[CH:11]=[C:3]2[C:4](=[CH:8][C:9]=1[O:14][CH3:15])[C:5](=[O:6])[O:7][CH:1]2[PH2:22]([C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1)([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

참가 물질

6

반응물 3

HCID 260Hydrogen BromideHCID 11776TriphenylphosphineHCID 71762072-Formyl-4,5-dimethoxybenzoic acid

생성물 0

아직 생성물 데이터가 없습니다.

시약·촉매·용매 3

HCID 176Acetic Acid용매2회HCID 3283Diethyl Ether용매HCID 6342Acetonitrile용매

반응 조건

온도
90 °C

실험 절차

A suspension of 2-formyl-4,5-dimethoxy-benzoic acid (6.43 g, 30.62 mmoles), obtained as described in example 2, triphenyl-phosphine (8.3 g, 30.62 mmoles), 30% HBr in acetic acid (8.26 ml, 30.62 mmoles) and glacial acetic acid (20 ml) under N2 was heated at 90° C. for 4.5 hours. The mixture was brought to dryness, re-dissolved in acetonitrile (50 ml) and diluted with ethyl ether up to turbidity, then cooled and filtered, and the filtrate was washed with ethyl ether and dried under vacuum to give 13.6 g of the title compound (yield: 83%).

후처리

  1. customobtained
  2. temperaturecooled
  3. filtrationfiltered
  4. washthe filtrate was washed with ethyl ether
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-cbbf3575b47045bca0481a74c07a90ae
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525055B1

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