Ammonium Chloride → HCID 68567915、化合物

HRID 2242146ノート

反応式

HRID 2242146 の反応式
C[Al](C)C.[C:5]([N:9]1[C:13]([NH2:14])=[CH:12][C:11]([CH:15]2[CH2:18][C:17]([O:21][CH3:22])([O:19][CH3:20])[CH2:16]2)=[N:10]1)([CH3:8])([CH3:7])[CH3:6].C([O:25][C:26](=O)[C:27]([CH3:35])([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=1)[CH3:28])C.[NH4+].[Cl-]>CCCCCCC.C(Cl)Cl>[C:5]([N:9]1[C:13]([NH:14][C:26](=[O:25])[C:27]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=2)([CH3:35])[CH3:28])=[CH:12][C:11]([CH:15]2[CH2:16][C:17]([O:19][CH3:20])([O:21][CH3:22])[CH2:18]2)=[N:10]1)([CH3:8])([CH3:7])[CH3:6]

参加物

7

反応物 4

HCID 25517Ammonium ChlorideHCID 642856Ethyl 2-methyl-2-(pyridin-2-yl)propanoateHCID 16682925TrimethylaluminumHCID 57525626HCID 57525626、化合物

生成物 1

HCID 68567915HCID 68567915、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 8900Heptane溶媒

実験手順

A solution of trimethylaluminum in heptane (2.0 M, 19.5 mL) was added slowly to a solution of 2-tert-butyl-5-(3,3-dimethoxy-cyclobutyl)-2H-pyrazol-3-ylamine (8.98 g) in CH2Cl2 (60 mL) at room temperature. After 15 min, a solution of 2-methyl-2-pyridin-2-yl-propionic acid ethyl ester (6.85 g) in CH2Cl2 (60 mL) was added. The reaction mixture was heated to reflux overnight. Saturated aqueous NH4Cl solution was added and the mixture was extracted with CH2Cl2 (2×). The combined organic layers were dried over Na2SO4 and concentrated to afford N-[2-tert-butyl-5-(3,3-dimethoxy-cyclobutyl)-2H-pyrazol-3-yl]-2-pyridin-2-yl-isobutyramide as an oil that was used without further purification.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux overnight
  3. extractionthe mixture was extracted with CH2Cl2 (2×)
  4. dry with materialThe combined organic layers were dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-21fbfc68c1b44d2eb08e9d91898f5dec
出典データセット
uspto-grants-2010_03
特許番号
US07671072B2

反応ノート

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