Chlorodifluoromethane → 4-Chloro-4'-difluoromethylthiomethyl-benzophenone

HRID 2098

反応式

HRID 2098 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.[OH-].[K+].O1CCOCC1.[F:26][CH:27](Cl)[F:28]>O>[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][CH:27]([F:28])[F:26])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 6372ChlorodifluoromethaneHCID 14797Potassium HydroxideHCID 312751,4-DioxaneHCID 196893804-Chloro-4'-mercaptomethylbenzophenone2 回

生成物 1

HCID 196893694-Chloro-4'-difluoromethylthiomethyl-benzophenone収率 36%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4-chloro-4'-mercaptomethylbenzophenone (14.7 g) and potassium hydroxide (15 g) was added to a solvent comprising dioxane (100 ml) and water (100 ml). Difluoromethyl chloride was blown into this solution at 60° C. until the starting material 4-chloro-4'-mercaptomethylbenzophenone disappeared. The reaction product was cooled to room temperature and then subjected to filtration. The organic layer as the filtrate was dried over anhydrous magnesium sulfate add concentrated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1) to obtain the desired product (6.4 g, melting point: 34° to 35° C., yield: 36%).

後処理

  1. filtrationsubjected to filtration
  2. dry with materialThe organic layer as the filtrate was dried over anhydrous magnesium sulfate
  3. additionadd
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1)

出典と根拠

ORDレコード
ord-54662bdd64d74fb6bcb38cb65a7a5fc0
出典データセット
uspto-grants-1998_03
特許番号
US05728699

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