tert-Butanol → tert-Butyl 2,4,5-trichlorophenyl carbonate

HRID 1730152

반응식

HRID 1730152 반응식
Cl[C:2]([O:4][C:5]1[CH:10]=[C:9]([Cl:11])[C:8]([Cl:12])=[CH:7][C:6]=1[Cl:13])=[O:3].[C:14]([OH:18])([CH3:17])([CH3:16])[CH3:15].N1C2C(=CC=CC=2)C=CC=1>C(Cl)Cl>[C:2](=[O:3])([O:4][C:5]1[CH:10]=[C:9]([Cl:11])[C:8]([Cl:12])=[CH:7][C:6]=1[Cl:13])[O:18][C:14]([CH3:17])([CH3:16])[CH3:15]

참가 물질

5

반응물 3

HCID 6386tert-ButanolHCID 7047QuinolineHCID 85650Carbonochloridic acid, 2,4,5-trichlorophenyl ester

생성물 1

HCID 86887tert-Butyl 2,4,5-trichlorophenyl carbonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

T-Butyl 2,4,5-trichlorophenyl carbonate is a known compound and one method for its preparation is described in an article by W. Broadbent, J. S. Morley and B. E. Stone in the Journal of the Chemical Society (C), 1967 pages 2632-2637. Briefly, in this method a solution of phosgene in toluene is treated with 2,4,5-trichlorophenol at -10° C, followed by addition of dimethylaniline at such a rate that the reaction temperature is maintained at 5°-10° C. The mixture is heated to 20°-24° C and maintained at this temperature for 12 hours. The mixture is cooled by addition of ice and the suspension filtered. From the organic layer in the filtrate, 2,4,5-trichlorophenyl chloroformate is isolated. A solution of the crude 2,4,5-trichlorophenyl chloroformate in methylene chloride is reacted with a solution of t-butanol and quinoline in methylene chloride. The reaction mixture is maintained at 20°-24° C for 12 hours. The mixture is cooled by addition of ice and the suspension is filtered. From the organic layer in the filtrate t-butyl 2,4,5-trichlorophenyl carbonate is isolated.

후처리

  1. temperatureThe reaction mixture is maintained at 20°-24° C for 12 hours
  2. temperatureThe mixture is cooled by addition of ice
  3. filtrationthe suspension is filtered

출처 및 근거

ORD 기록
ord-7a878406cf214f479336e843ab2f5754
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03991205

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