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

HRID 2098

반응식

HRID 2098 반응식
[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

참가 물질

6

반응물 4

HCID 6372ChlorodifluoromethaneHCID 14797Potassium HydroxideHCID 312751,4-DioxaneHCID 196893804-Chloro-4'-mercaptomethylbenzophenone2회

생성물 1

HCID 196893694-Chloro-4'-difluoromethylthiomethyl-benzophenone수율 36%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-54662bdd64d74fb6bcb38cb65a7a5fc0
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728699

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