4'-Hydroxypropiophenone → Ifenprodil hydrobromide

HRID 355077

反応式

HRID 355077 の反応式
O1CCOCC1.[OH:7][C:8]1[CH:13]=[CH:12][C:11]([C:14](=[O:17])[CH2:15][CH3:16])=[CH:10][CH:9]=1.[Br:18]Br.[CH2:20]([C:27]1[CH:32]=[CH:31][N:30]=[CH:29][CH:28]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>CO>[CH3:16][CH:15]([N:30]1[CH2:31][CH2:32][CH:27]([CH2:20][C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH2:28][CH2:29]1)[CH:14]([OH:17])[C:11]1[CH:12]=[CH:13][C:8]([OH:7])=[CH:9][CH:10]=1.[BrH:18]

参加物

6

反応物 4

HCID 62714'-HydroxypropiophenoneHCID 164584-BenzylpyridineHCID 24408BromineHCID 312751,4-Dioxane

生成物 1

HCID 12613162Ifenprodil hydrobromide収率 70.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a mixture of 3 ml of dioxane and 1 ml of methanol were added 6.0 g of 4'-hydroxypropiophenone. 6.4 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 400 ml/minute for 15 minutes at 60° C. To the reaction 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. The reaction mixture was then treated in the same manner as described in Example 5, whereby 11.4 g (70.4%) of ifenprodil hydrobromide 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. customTo the reaction liquid
  5. temperaturethe mixture was refluxed
  6. temperatureunder heating for 5 hours
  7. additionThe reaction mixture was then treated in the same manner

出典と根拠

ORDレコード
ord-dfa6965e2cfe46519d388a62cab50ded
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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