Potassium Acetate → HCID 178494125、化合物

HRID 474766ノート

反応式

HRID 474766 の反応式
Cl.[Cl:2][C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16](=[NH:18])[NH2:17])=[CH:10][CH:9]=2)=[CH:5][C:4]=1[C:21]([F:24])([F:23])[F:22].[OH:25][CH:26]=[C:27]([CH2:32][C:33]1[CH:34]=[N:35][C:36]([O:39][CH3:40])=[N:37][CH:38]=1)[C:28](OC)=O.C([O-])(=O)C.[K+]>C1(C)C=CC=CC=1>[Cl:2][C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16]3[NH:17][CH:28]=[C:27]([CH2:32][C:33]4[CH:34]=[N:35][C:36]([O:39][CH3:40])=[N:37][CH:38]=4)[C:26](=[O:25])[N:18]=3)=[CH:10][CH:9]=2)=[CH:5][C:4]=1[C:21]([F:22])([F:23])[F:24]

参加物

5

反応物 3

HCID 517044Potassium AcetateHCID 67773588Methyl 3-hydroxy-2-((2-methoxypyrimidin-5-yl)methyl)acrylateHCID 677756383-(4-(4-Chloro-3-(trifluoromethyl)phenoxy)phenyl)propanimidamide hydrochloride

生成物 1

HCID 178494125HCID 178494125、化合物収率 42.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

The suspension of 3-(4-(4-chloro-3-(trifluoromethyl)phenoxy)phenyl)propanimidamide hydrochloride (5.9 g, 15.56 mmol), methyl 3-hydroxy-2-((2-methoxypyrimidin-5-yl)methyl)acrylate (3.49 g, 15.56 mmol) and potassium acetate (4.58 g, 46.7 mmol) in toluene (100 mL) was heated under reflux overnight. Dean-Stark apparatus was used to remove water formed in the reaction. The residue was recrystallized in ethyl acetate and washed with ether to provide the title compound (3.4 g, 42%). LCMS: rt=1.71 min, [M+H+]=517

後処理

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. customto remove water
  4. customformed in the reaction
  5. customThe residue was recrystallized in ethyl acetate
  6. washwashed with ether

出典と根拠

ORDレコード
ord-3c4da1d8fdd24e45bbf75479c47b4876
出典データセット
uspto-grants-2014_01
特許番号
US08637536B2

反応ノート

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