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Ammonium Acetate → HCID 178442439, 화합물

HRID 425398
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HRID 425398 반응식
C([O-])(=O)C.[NH4+:5].[C:6]([NH:9][CH:10]([C:32]([NH:34][CH2:35][C:36](=O)[CH2:37][C:38]([CH3:42])([CH3:41])[CH2:39][CH3:40])=O)[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[C:19]([NH:24][C:25](=[O:31])[O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[N:20][N:21]([CH3:23])[CH:22]=2)=[CH:14][CH:13]=1)(=[O:8])[CH3:7]>C1(C)C(C)=CC=CC=1>[C:27]([O:26][C:25](=[O:31])[NH:24][C:19]1[C:18]([C:15]2[CH:16]=[CH:17][C:12]([CH2:11][CH:10]([NH:9][C:6](=[O:8])[CH3:7])[C:32]3[NH:34][CH:35]=[C:36]([CH2:37][C:38]([CH3:41])([CH3:42])[CH2:39][CH3:40])[N:5]=3)=[CH:13][CH:14]=2)=[CH:22][N:21]([CH3:23])[N:20]=1)([CH3:29])([CH3:30])[CH3:28]
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참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 86637804tert-butyl [4-(4-{2-(acetylamino)-3-[(4,4-dimethyl-2-oxohexyl)amino]-3-oxopropyl}phenyl)-1-methyl-1H-pyrazol-3-yl]carbamate

생성물 1

HCID 178442439HCID 178442439, 화합물

시약·촉매·용매 1

HCID 7237O-Xylene용매

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온도
150 °C

실험 절차

Ammonium acetate (1.17 g, 15.2 mmol) was added to an ambient temperature solution of tert-butyl [4-(4-{2-(acetylamino)-3-[(4,4-dimethyl-2-oxohexyl)amino]-3-oxopropyl}phenyl)-1-methyl-1H-pyrazol-3-yl]carbamate (160 mg, 0.30 mmol) in xylene (5 mL). After stirring at 150° C. for 1 h, the reaction mixture was quenched with saturated aqueous sodium bicarbonate and extracted with ethyl acetate and methylene chloride. The combined organic extracts were dried (magnesium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-100% acetone/methylene chloride afforded the title compound. (M+H) found: 509.

후처리

  1. customthe reaction mixture was quenched with saturated aqueous sodium bicarbonate
  2. extractionextracted with ethyl acetate and methylene chloride
  3. dry with materialThe combined organic extracts were dried (magnesium sulfate)
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-726f36e91fc0455bbc4b32a1386186c0
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106070B2

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