Potassium Carbonate → HCID 18504562、化合物

HRID 1387233ノート

反応式

HRID 1387233 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-ea7029312780451a9bb93b65eaa437a7
出典データセット
uspto-grants-2001_07
特許番号
US06268313B1

反応ノート

読み込み中…