4'-Hydroxypropiophenone → Ifenprodil

HRID 355086

反応式

HRID 355086 の反応式
C(OCCCC)CCC.[OH:10][C:11]1[CH:16]=[CH:15][C:14]([C:17](=[O:20])[CH2:18][CH3:19])=[CH:13][CH:12]=1.BrBr.[CH2:23]([C:30]1[CH:35]=[CH:34][N:33]=[CH:32][CH:31]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CO>[CH3:19][CH:18]([N:33]1[CH2:34][CH2:35][CH:30]([CH2:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH2:31][CH2:32]1)[CH:17]([OH:20])[C:14]1[CH:15]=[CH:16][C:11]([OH:10])=[CH:12][CH:13]=1

参加物

6

反応物 4

HCID 62714'-HydroxypropiophenoneHCID 8909Butyl etherHCID 164584-BenzylpyridineHCID 24408Bromine

生成物 1

HCID 3689Ifenprodil収率 86.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 15 ml of di-n-butyl ether were added 6.0 g of 4'-hydroxypropiophenone. 6.6 Grams of bromine were added dropwise to the mixture with stirring at room temperature. The reaction liquid was stirred for an additional 10 minutes and then nitrogen was introduced thereinto at a flow rate of 200 ml/minute for one hour at room temperature. To the treaction liquid were then added 7.5 g of 4-benzylpyridine and 100 ml of methanol, and the mixture was refluxed under heating for 5 hours. After stopping the heating, the reaction mixture was treated in the same manner as described in Example 35, whereby 11.3 g (73.4%) of ifenprodil were obtained as white crystals.

後処理

  1. customThe reaction liquid
  2. stirringwas stirred for an additional 10 minutes
  3. additionnitrogen was introduced
  4. temperaturethe mixture was refluxed
  5. temperatureunder heating for 5 hours
  6. additionthe reaction mixture was treated in the same manner

出典と根拠

ORDレコード
ord-32383a483a3546a4a3726561f3d84def
出典データセット
uspto-grants-1983_03
特許番号
US04377691

関連ノート

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