Ammonium Chloride → HCID 68567915, 화합물

HRID 2242146노트

반응식

HRID 2242146 반응식
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]

참가 물질

7

반응물 4

HCID 25517Ammonium ChlorideHCID 642856Ethyl 2-methyl-2-(pyridin-2-yl)propanoateHCID 16682925TrimethylaluminumHCID 57525626HCID 57525626, 화합물

생성물 1

HCID 68567915HCID 68567915, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 8900Heptane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-21fbfc68c1b44d2eb08e9d91898f5dec
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07671072B2

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