Hydrogen Bromide →

HRID 1060578

反応式

HRID 1060578 の反応式
[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

参加物

6

反応物 3

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

生成物 0

生成物のデータはまだありません。

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒2 回HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
90 °C

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-cbbf3575b47045bca0481a74c07a90ae
出典データセット
uspto-grants-2003_02
特許番号
US06525055B1

関連ノート

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