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Hydrochloric Acid → HCID 136346604, 화합물

HRID 1931779
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HRID 1931779 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:18]3=[N:19][C:20]([O:25][CH3:26])=[N:21][C:22]([O:23]C)=[C:17]3[CH:16]=[N:15]2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].O1CCOCC1.Cl>O.C(OCC)(=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:18]3[N:19]=[C:20]([O:25][CH3:26])[NH:21][C:22](=[O:23])[C:17]=3[CH:16]=[N:15]2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 312751,4-DioxaneHCID 66915353HCID 66915353, 화합물

생성물 1

HCID 136346604HCID 136346604, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 8857
Ethyl Acetate
용매

반응 조건

온도
40 °C

실험 절차

A mixture of 4-(4,6-dimethoxy-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester (1 mmol), 2 M aqueous sodium hydroxide (1 mL) and dioxane (10 mL) is heated at 40° C. for 5 h. The mixture is allowed to cool, and is then neutralized to approximately pH 7 by the addition of 1 M aqueous hydrochloric acid. Ethyl acetate and water are added. The organic layer is washed with water and brine, dried (magnesium sulfate), filtered, evaporated, and purified by flash chromatography on silica gel to give 4-(6-methoxy-4-oxo-4,5-dihydro-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester.

후처리

  1. temperatureto cool
  2. washThe organic layer is washed with water and brine
  3. dry with materialdried (magnesium sulfate)
  4. filtrationfiltered
  5. customevaporated
  6. custompurified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-090160b96655448090a4eb32cf3a9c47
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08188098B2

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