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Methanol → 4-Chloro-4'-ethylthiomethylbenzophenone

HRID 1421545
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HRID 1421545 반응식
[Br-].[Cl:2][C:3]1[CH:21]=[CH:20][C:6]([C:7]([C:9]2[CH:19]=[CH:18][C:12]([CH2:13][S:14][C:15](N)=[NH2+])=[CH:11][CH:10]=2)=[O:8])=[CH:5][CH:4]=1.[C:22](=O)([O-])[O-].[K+].[K+].CO.[OH-].[K+]>C1(C)C=CC=CC=1.O>[Cl:2][C:3]1[CH:21]=[CH:20][C:6]([C:7]([C:9]2[CH:19]=[CH:18][C:12]([CH2:13][S:14][CH2:15][CH3:22])=[CH:11][CH:10]=2)=[O:8])=[CH:5][CH:4]=1
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참가 물질

7

반응물 4

HCID 887MethanolHCID 11430Potassium CarbonateHCID 14797Potassium HydroxideHCID 18779877S-(4-(4-chlorobenzoyl)benzyl)thiouronium bromide

생성물 1

HCID 196893544-Chloro-4'-ethylthiomethylbenzophenone수율 52.2%

시약·촉매·용매 2

HCID 962Water
용매
HCID 1140Toluene용매

실험 절차

S-(4-(4-chlorobenzoyl)benzyl)thiouronium bromide (3.3 g) and potassium carbonate (1.5 g) were dissolved in dimethylformnamide (20 ml). A methanol solution (10 ml) of potassium hydroxide (1.0 g) was added and stirred at room temperature for 30 minutes. To the reaction mixture, water (100 ml) and toluene (100 ml) were added. The organic layer was separated, and washed with water and an aqueous saturated sodium chloride solution, followed by drying over anhydrous magnesium sulfate. After distilling off the solvent, the crude product was purified by silica gel column chromatography (developing solvent: ethyl acetaten:hexane=1:9) to obtain 4-chloro-4'-ethylmercaptomethylbenzophenone (1.3 g).

후처리

  1. customThe organic layer was separated
  2. washwashed with water
  3. dry with materialby drying over anhydrous magnesium sulfate
  4. distillationAfter distilling off the solvent
  5. customthe crude product was purified by silica gel column chromatography (

출처 및 근거

ORD 기록
ord-54e40a5d942344f9a6b07f05d96c6218
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06077866

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