Ammonium Acetate → 2-benzyloxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazole

HRID 1416008ノート

反応式

HRID 1416008 の反応式
C([O-])(=O)C.[NH4+:5].[CH2:6]([O:13][CH2:14][C:15]([N:17]([CH:19]([S:25][C:26]1[CH:31]=[C:30]([Cl:32])[CH:29]=[C:28]([Cl:33])[CH:27]=1)[C:20](=O)[CH:21]([CH3:23])[CH3:22])[CH3:18])=O)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)(=O)C>[CH2:6]([O:13][CH2:14][C:15]1[N:17]([CH3:18])[C:19]([S:25][C:26]2[CH:31]=[C:30]([Cl:32])[CH:29]=[C:28]([Cl:33])[CH:27]=2)=[C:20]([CH:21]([CH3:23])[CH3:22])[N:5]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 221306862-benzyloxy-N-[1-(3,5-dichlorophenylthio)-3-methyl-2-oxobutyl]-N-methylacetamide

生成物 1

HCID 221305032-benzyloxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazole

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

In acetic acid was dissolved 2-benzyloxy-N-[1-(3,5-dichlorophenylthio)-3-methyl-2-oxobutyl]-N-methylacetamide (20), followed by addition of ammonium acetate, and the mixture was refluxed under heating. After 1 hour, the reaction mixture was concentrated under reduced pressure, neutralized with sodium hydroxide, and then, extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated to give 2-benzyloxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1H-methylimidazole (17a).

後処理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-9cbc54a4154e40f3b5711277c790668d
出典データセット
uspto-grants-1999_06
特許番号
US05910506

反応ノート

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