Methanol → Ifenprodil hydrobromide

HRID 355076

반응식

HRID 355076 반응식
CO.[OH:3][C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:13])[CH2:11][CH3:12])=[CH:6][CH:5]=1.[Br:14]Br.[CH2:16]([C:23]1[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C(O)C>[CH3:12][CH:11]([N:26]1[CH2:27][CH2:28][CH:23]([CH2:16][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH2:24][CH2:25]1)[CH:10]([OH:13])[C:7]1[CH:8]=[CH:9][C:4]([OH:3])=[CH:5][CH:6]=1.[BrH:14]

참가 물질

6

반응물 4

HCID 887MethanolHCID 62714'-HydroxypropiophenoneHCID 164584-BenzylpyridineHCID 24408Bromine

생성물 1

HCID 12613162Ifenprodil hydrobromide수율 65.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 5 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 air was introduced thereinto at a flow rate of 200 ml/minute for 30 minutes at room temperature. To the reaction liquid were then added 7.5 g of 4-benzylpyridine and 100 ml of ethanol, and the mixture was refluxed under heating for 5 hours. The reaction mixture was treated in the same manner as described in Example 5, whereby 10.7 g (65.8%) of ifenprodil hydrobromide were obtained as white crystals.

후처리

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

출처 및 근거

ORD 기록
ord-f3f83a38be1b4b6891216f27cbc38c49
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04377691

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