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Water → HCID 117864549, 화합물

HRID 1486355
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HRID 1486355 반응식
C(OC(=O)[NH:7][C:8]([CH3:36])([CH2:33][CH2:34][CH3:35])[CH2:9][NH:10][C:11]([C:13]1[C:14]([CH3:32])=[N:15][N:16]2[C:21]([O:22][CH2:23][C:24]3[C:29]([F:30])=[CH:28][CH:27]=[CH:26][N:25]=3)=[CH:20][C:19]([CH3:31])=[CH:18][C:17]=12)=[O:12])(C)(C)C.O.[OH-].[Na+]>FC(F)(F)C(O)=O>[NH2:7][C:8]([CH3:36])([CH2:33][CH2:34][CH3:35])[CH2:9][NH:10][C:11]([C:13]1[C:14]([CH3:32])=[N:15][N:16]2[C:21]([O:22][CH2:23][C:24]3[C:29]([F:30])=[CH:28][CH:27]=[CH:26][N:25]=3)=[CH:20][C:19]([CH3:31])=[CH:18][C:17]=12)=[O:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

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HCID 962WaterHCID 14798Sodium HydroxideHCID 117864682rac-{1-[({7-[(3-Fluoropyridin-2-yl)methoxy]-2,5-dimethylpyrazolo[1,5-a]pyridin-3-yl}carbonyl)amino]-2-methylpentan-2-yl}carbamic Acid tert-butyl Ester

생성물 1

HCID 117864549HCID 117864549, 화합물수율 10%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

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온도
50 °C

실험 절차

20 mg (0.039 mmol) of rac-{1-[({7-[(3-fluoropyridin-2-yl)methoxy]-2,5-dimethylpyrazolo[1,5-a]pyridin-3-yl}carbonyl)amino]-2-methylpentan-2-yl}carbamic acid tert-butyl ester (Example 144A) were dissolved in 1 ml of trifluoroacetic acid. The reaction mixture was heated to 50° C. for 1 hour. Water was added, and the pH was adjusted to −9 with 2 N sodium hydroxide solution. The aqueous phase was extracted with dichloromethane, separated off and concentrated under reduced pressure. The residue was purified by preparative HPLC chromatography (Method 21), which gave 1.59 mg (10% yield) of the target compound.

후처리

  1. extractionThe aqueous phase was extracted with dichloromethane
  2. customseparated off
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by preparative HPLC chromatography (Method 21), which

출처 및 근거

ORD 기록
ord-7256099ea0c543a9a62d014201b7d3f1
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09422285B2

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