Phosphorus oxychloride → HCID 178489920、化合物

HRID 599594ノート

反応式

HRID 599594 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:12]2[NH:16][C:15](/[CH:17]=[CH:18]/[C:19]3[CH:24]=[CH:23][C:22]([N:25]4[CH:29]=[C:28]([CH3:30])[N:27]=[CH:26]4)=[C:21]([O:31][CH3:32])[CH:20]=3)=[N:14][N:13]=2)[CH2:9][CH2:10]O)=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:35])=O>>[Cl:35][CH2:10][CH2:9][CH:8]([C:12]1[NH:16][C:15](/[CH:17]=[CH:18]/[C:19]2[CH:24]=[CH:23][C:22]([N:25]3[CH:29]=[C:28]([CH3:30])[N:27]=[CH:26]3)=[C:21]([O:31][CH3:32])[CH:20]=2)=[N:14][N:13]=1)[C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1

参加物

3

実験手順

A solution of 3-(4-fluorophenyl)-3-{5-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-4H-[1,2,4]triazol-3-yl}propan-1-ol (83 mg) in phosphorus oxychloride (1 mL) was stirred at 120° C. for one hour. The reaction solution was left to cool to room temperature and then concentrated under reduced pressure. Ethyl acetate and saturated sodium bicarbonate water were added to the residue, and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 86 mg of the title compound. The property value of the compound is as follows.

後処理

  1. waitThe reaction solution was left
  2. concentrationconcentrated under reduced pressure
  3. additionEthyl acetate and saturated sodium bicarbonate water were added to the residue
  4. customthe organic layer was separated
  5. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d99dbc4ee5054495977630087d9422cf
出典データセット
uspto-grants-2011_03
特許番号
US07897632B2

反応ノート

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