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1,1-Dichloroethane → Chloromethyl 3-trifluoromethoxybenzoate

HRID 1880753
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HRID 1880753 반응식
Cl[CH:2]([Cl:4])C.[F:5][C:6]([F:18])([F:17])[O:7][C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11](Cl)=[O:12].[O:19]1CCCOO1>[Cl-].[Cl-].[Cl-].[Cl-].[Zr+4].O>[F:5][C:6]([F:18])([F:17])[O:7][C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11]([O:19][CH2:2][Cl:4])=[O:12]
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참가 물질

6

반응물 3

HCID 63651,1-DichloroethaneHCID 5228543-(Trifluoromethoxy)benzoyl chlorideHCID 19593658CID 19593658

생성물 1

HCID 59570317Chloromethyl 3-trifluoromethoxybenzoate

시약·촉매·용매 2

HCID 9856075Zirconium chloride (ZrCl4), (T-4)-촉매HCID 962Water용매

실험 절차

To 10 ml of dichloroethane were added 0.93 g of zirconium tetrachloride and 1 g of 3-trifluoromethoxybenzoyl chloride, and the mixture was stirred at room temperature for 20 minutes. At 10° C., 0.15 g of trioxane was added, and the mixture was stirred for 30 minutes, and further stirred at room temperature for 1 hour. Water was added slowly under ice-cooling, the resultant solution was extracted with chloroform three times, and the organic layers were combined, washed with an aqueous saturated sodium bicarbonate solution and an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated to obtain 1 g of chloromethyl 3-trifluoromethoxybenzoate.

후처리

  1. stirringthe mixture was stirred for 30 minutes
  2. stirringfurther stirred at room temperature for 1 hour
  3. temperaturecooling
  4. extractionthe resultant solution was extracted with chloroform three times
  5. washwashed with an aqueous saturated sodium bicarbonate solution
  6. dry with materialan aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-57d8e3e9dbf74feaa69d6a3faf47a6cb
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318776B2

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