Potassium Carbonate → HCID 53643449、化合物

HRID 363061ノート

反応式

HRID 363061 の反応式
[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]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 173781,1,3-TrichloropropeneHCID 54015144HCID 54015144、化合物

生成物 1

HCID 53643449HCID 53643449、化合物収率 82%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b0c8cf2550c147f08410b9d2dcfe3e77
出典データセット
uspto-grants-1999_02
特許番号
US05872137

反応ノート

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