Potassium Carbonate → HCID 18504562、化合物

HRID 582332ノート

反応式

HRID 582332 の反応式
[CH2:1]([C:3]1[CH:4]=[C:5]([OH:25])[CH:6]=[C:7]([CH3:24])[C:8]=1[O:9][CH2:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][N:15]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[Cl:32][C:33]([Cl:37])=[CH:34][CH2:35]Cl>CN(C)C=O>[CH2:1]([C:3]1[CH:4]=[C:5]([O:25][CH2:35][CH:34]=[C:33]([Cl:37])[Cl:32])[CH:6]=[C:7]([CH3:24])[C:8]=1[O:9][CH2:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([F:22])([F:21])[F:23])=[CH:16][N:15]=1)[CH3:2]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 173781,1,3-TrichloropropeneHCID 18504580HCID 18504580、化合物

生成物 1

HCID 18504562HCID 18504562、化合物収率 65.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

In 10 ml of N,N-dimethylformamide were dissolved 0.7 g of 3-ethyl-5-methyl-4-[3-(5-trifluoromethyl-2-pyridyloxy)propyloxy]phenol and 0.27 g of potassium carbonate, to which a solution of 0.34 g of 1,1,3-trichloropropene dissolved in 5 ml of N,N-dimethylformamide was added dropwise, while stirring at room temperature. After stirring at room temperature for 12 hours, the reaction mixture was poured into ice-water, and extracted twice with 100 ml of diethyl ether. The combined diethyl ether was washed with water, dried with anhydrous magnesium sulfate, and concentrated to obtain a crude product. The crude produce was subjected to silica gel chromatography, which afforded 0.6 g of 3-ethyl-5-methyl-4-[3-(5-trifluoromethyl-2-pyridyloxy)propyloxy]-1-(3,3-dichloro-2-propenyloxy)benzene (65% yield), nD23.0 1.5188.

後処理

  1. additionwas added dropwise
  2. stirringAfter stirring at room temperature for 12 hours
  3. extractionextracted twice with 100 ml of diethyl ether
  4. washThe combined diethyl ether was washed with water
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customto obtain a crude product
  8. customThe crude produce

出典と根拠

ORDレコード
ord-7b639642f2db418b8468b614665ded77
出典データセット
uspto-grants-1999_07
特許番号
US05922880

反応ノート

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