Potassium Carbonate → HCID 53643449, 화합물

HRID 363061노트

반응식

HRID 363061 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([OH:16])[CH:5]=[C:6]([Cl:15])[C:7]=1[O:8][C:9]([F:14])([F:13])[CH:10]([F:12])[F:11].C(=O)([O-])[O-].[K+].[K+].[Cl:23][C:24]([Cl:28])=[CH:25][CH2:26]Cl>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([O:16][CH2:26][CH:25]=[C:24]([Cl:28])[Cl:23])[CH:5]=[C:6]([Cl:15])[C:7]=1[O:8][C:9]([F:14])([F:13])[CH:10]([F:12])[F:11]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 173781,1,3-TrichloropropeneHCID 54015144HCID 54015144, 화합물

생성물 1

HCID 53643449HCID 53643449, 화합물수율 82%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a mixture of 600 mg of 3,5-dichloro-4-(1,1,2,2-tetrafluoroethoxy)phenol, 330 mg of potassium carbonate and 10 ml of N,N-dimethylformamide was added dropwise a solution of 340 mg of 1,1,3-trichloro-1-propene dissolved in 3 ml of N,N-dimethylformamide, while stirring at room temperature. After stirring continued at room temperature for 5 hours, the reaction mixture was poured into ice-water, and extracted twice with 40 ml of diethyl ether. The combined ether layer was washed with water, dried with anhydrous magnesium sulfate, and concentrated to obtain a crude product. The crude product was subjected to silica gel chromatography, which afforded 630 mg of 3,5-dichloro-4-(1,1,2,2-tetrafluoroethoxy)-1-(3,3-dichloro-2-propenyloxy)benzene (82% yield), nD24.6 1.5067.

후처리

  1. stirringAfter stirring
  2. extractionextracted twice with 40 ml of diethyl ether
  3. washThe combined ether layer was washed with water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customto obtain a crude product

출처 및 근거

ORD 기록
ord-b0c8cf2550c147f08410b9d2dcfe3e77
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05872137

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