Ethyl Bromide → 4-Chloro-4'-ethylthiomethylbenzophenone

HRID 2097

反応式

HRID 2097 の反応式
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][SH:15])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.[CH2:18](Br)[CH3:19].[OH-].[K+]>CO>[Cl:1][C:2]1[CH:17]=[CH:16][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][S:15][CH2:18][CH3:19])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 6332Ethyl BromideHCID 14797Potassium HydroxideHCID 196893804-Chloro-4'-mercaptomethylbenzophenone

生成物 1

HCID 196893544-Chloro-4'-ethylthiomethylbenzophenone収率 79.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4-chloro-4'-mercaptomethylbenzophenone (16.0 g), ethyl bromide (7.4 g) and potassium hydroxide (4.3 g) were added to methanol (250 ml), and the mixture was stirred for 30 minutes under reflux. The reaction mixture was cooled to room temperature and then concentrated. Water was added to the residue, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1) to obtain the desired product 14.0 g, melting point: 33° to 34° C., yield: 79%).

後処理

  1. temperatureunder reflux
  2. concentrationconcentrated
  3. additionWater was added to the residue
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated
  8. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-854622046616431a8dec648c46bb4905
出典データセット
uspto-grants-1998_03
特許番号
US05728699

関連ノート

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