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Thionyl Chloride → HCID 68352149、化合物

HRID 2174552
ノート
印刷プレビュー

反応式

HRID 2174552 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[N:7][N:8]([CH2:10][C:11]([OH:13])=O)[CH:9]=1)=[O:4].S(Cl)(Cl)=O.[NH2:18][C:19]1[CH:24]=[C:23]([Cl:25])[C:22]([C:26]2[CH:31]=[CH:30][C:29]([N:32]3[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]3)=[CH:28][CH:27]=2)=[CH:21][C:20]=1[C:38]([O:40][CH3:41])=[O:39]>C1(C)C=CC=CC=1.ClCCl>[Cl:25][C:23]1[CH:24]=[C:19]([NH:18][C:11](=[O:13])[CH2:10][N:8]2[CH:9]=[C:5]([C:3]([O:2][CH3:1])=[O:4])[CH:6]=[N:7]2)[C:20]([C:38]([O:40][CH3:41])=[O:39])=[CH:21][C:22]=1[C:26]1[CH:27]=[CH:28][C:29]([N:32]2[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]2)=[CH:30][CH:31]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 24386Thionyl ChlorideHCID 19576734[4-(methoxycarbonyl)-1H-pyrazol-1-yl]acetic acidHCID 68352047HCID 68352047、化合物2 回

生成物 1

HCID 68352149HCID 68352149、化合物収率 97.2%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344
Dichloromethane
溶媒

反応条件

温度
90 °C

実験手順

To a solution of 2-(4-(methoxycarbonyl)-1H-pyrazol-1-yl)acetic acid (ChemCollect GmbH, 401 mg, 2.175 mmol) in toluene (10 mL) was added thionyl chloride (0.317 mL, 4.35 mmol) and the reaction mixture was stirred at 90° C. for 2 h. The solvent was removed under reduced pressure and the residue was added to a solution of methyl 4-amino-6-chloro-4′-(piperidin-1-yl)-[1,1′-biphenyl]-3-carboxylate (Intermediate 48) (500 mg, 1.45 mmol) in dichloromethane (10 mL). The reaction mixture was stirred at room temperature overnight. Solvent was removed under reduced pressure and water was added. Precipitate was observed, solid was filtered and dried to give the title compound methyl 1-(2-((2-chloro-5-(methoxycarbonyl)-4′-(piperidin-1-yl)-[1,1′-biphenyl]-4-yl)amino)-2-oxoethyl)-1H-pyrazole-4-carboxylate (720 mg, 1.409 mmol, 97% yield) as a cream solid. LCMS: (M+H)+=511; Rt=4.04 min.

後処理

  1. customThe solvent was removed under reduced pressure
  2. stirringThe reaction mixture was stirred at room temperature overnight
  3. customSolvent was removed under reduced pressure and water
  4. additionwas added
  5. filtrationsolid was filtered
  6. customdried

出典と根拠

ORDレコード
ord-273341e8e9454b4a842a380b9b47784c
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09061998B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート