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Sodium Hydroxide → HCID 10287414, 화합물

HRID 1437158
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HRID 1437158 반응식
C[O:2][C:3](=[O:30])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH2:10][N:11]2[CH2:16][CH2:15][CH:14]([C:17]3[C:25]4[C:20](=[N:21][CH:22]=[CH:23][CH:24]=4)[N:19]([CH2:26][CH2:27][O:28][CH3:29])[CH:18]=3)[CH2:13][CH2:12]2)[CH:5]=1.[OH-].[Na+]>C(O)C>[CH3:29][O:28][CH2:27][CH2:26][N:19]1[C:20]2=[N:21][CH:22]=[CH:23][CH:24]=[C:25]2[C:17]([CH:14]2[CH2:15][CH2:16][N:11]([CH2:10][C:6]3[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=3)[C:3]([OH:30])=[O:2])[CH2:12][CH2:13]2)=[CH:18]1
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 68896791HCID 68896791, 화합물

생성물 1

HCID 10287414HCID 10287414, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.66 g (1.62 mmol) of 3-{4-[1-(2-methoxyethyl)-1H-pyrrolo[2,3-b]pyridin-3-yl]-piperidin-1-ylmethyl}-benzoic acid methyl ester were dissolved in 0.8 ml of ethyl alcohol and 2.43 ml of 2 N sodium hydroxide were added. After stirring at room temperature for 20 hours, the solvent was evaporated under reduced pressure and the residue dissolved in water. The mixture was neutralised with 2 N hydrochloric acid and extracted twice with dichlormethane. The organic phase was washed with water and brine, dried with magnesium sulphate, filtrated and evaporated. The crude material weighed 0.46 g and was purified by flash chromatography over silica gel affording 0.2 g (31% of yield) of the expected product.

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. dissolutionthe residue dissolved in water
  3. extractionextracted twice with dichlormethane
  4. washThe organic phase was washed with water and brine
  5. dry with materialdried with magnesium sulphate
  6. filtrationfiltrated
  7. customevaporated
  8. customwas purified by flash chromatography over silica gel affording 0.2 g (31% of yield) of the expected product

출처 및 근거

ORD 기록
ord-d1a1a27850b541a9a5fd2fc3ac0b2927
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07622480B2

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