Acetone → {[(2-Methyl-1-nitropropan-2-yl)sulfanyl]methyl}benzene

HRID 1033822ノート

反応式

HRID 1033822 の反応式
[CH3:1][C:2]([CH3:4])=O.[CH2:5]([SH:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[N+:13]([CH3:16])([O-:15])=[O:14].N1CCCCC1>C1C=CC=CC=1.O>[CH2:5]([S:12][C:2]([CH3:4])([CH3:1])[CH2:16][N+:13]([O-:15])=[O:14])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

参加物

7

反応物 4

HCID 180AcetoneHCID 6375NitromethaneHCID 7509Benzyl mercaptanHCID 8082Piperidine

生成物 1

HCID 14613816{[(2-Methyl-1-nitropropan-2-yl)sulfanyl]methyl}benzene

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 962Water溶媒

実験手順

Acetone (25 g), benzyl mercaptan (53 g), nitromethane (26.2 g), and piperidine (8 cm3) were dissolved in benzene (150 cm3) and the mixture heated under reflux with azeotropic removal of water. After 48 h the reaction mixture was allowed to cool and washed first with dilute hydrochloric acid, then with water. The remaining solution was dried (MgSO4) and the solvent then removed under reduced pressure to give the nitro system (76.5 g, 85%). This material was sufficiently pure to be used without further purification.

後処理

  1. temperaturethe mixture heated
  2. temperatureto cool
  3. washwashed first with dilute hydrochloric acid
  4. dry with materialThe remaining solution was dried (MgSO4)
  5. customthe solvent then removed under reduced pressure

出典と根拠

ORDレコード
ord-f1507ad9f5b4440ba0987a3e0f60a33b
出典データセット
uspto-grants-1994_05
特許番号
US05312904

反応ノート

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