Sodium Chromate → 4-(3,5-Dichlorophenylmethyl)cyclohexanone

HRID 727165

반응식

HRID 727165 반응식
[Cr]([O-])([O-])(=O)=O.[Na+].[Na+].[Cl:8][C:9]1[CH:10]=[C:11]([CH2:16][CH:17]2[CH2:22][CH2:21][CH:20]([OH:23])[CH2:19][CH2:18]2)[CH:12]=[C:13]([Cl:15])[CH:14]=1>C(OCC)C>[Cl:8][C:9]1[CH:10]=[C:11]([CH2:16][CH:17]2[CH2:22][CH2:21][C:20](=[O:23])[CH2:19][CH2:18]2)[CH:12]=[C:13]([Cl:15])[CH:14]=1

참가 물질

4

반응물 2

HCID 24488Sodium ChromateHCID 197052214-(3,5-Dichlorophenylmethyl)cyclohexanol

생성물 1

HCID 197052684-(3,5-Dichlorophenylmethyl)cyclohexanone수율 36.1%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A solution of chromic acid was prepared using 5.6 grams of sodium dichromate, 16.8 mL of water, 4.1 mL of concentrated sulfuric acid, and additional water to provide 28 mL of solution. The sodium chromate solution was cooled to 0° C. and was added dropwise to a stirred, cold (0° C.) solution of 7.3 grams (0.028 mole) of 4-(3,5-dichlorophenylmethyl)cyclohexanol in 15 mL of diethyl ether. The complete addition required about 5 minutes. Upon completion of addition, the reaction mixture was stirred for 5 minutes and then was extracted with diethyl ether. The ether extract was washed with an aqueous solution saturated with sodium bicarbonate, then with water. The organic layer was concentrated under reduced pressure, yielding 2.6 grams of 4-(3,5-dichlorophenylmethyl)cyclohexanone.

후처리

  1. additionThe complete addition required about 5 minutes
  2. additionUpon completion of addition
  3. extractionwas extracted with diethyl ether
  4. extractionThe ether extract
  5. washwas washed with an aqueous solution saturated with sodium bicarbonate
  6. concentrationThe organic layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e3d06a9f5a66428e9a8fed0fd0be5ceb
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05712281

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