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Sodium Hydroxide → HCID 10287414、化合物

HRID 1437158
ノート
印刷プレビュー

反応式

HRID 1437158 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 68896791HCID 68896791、化合物

生成物 1

HCID 10287414HCID 10287414、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d1a1a27850b541a9a5fd2fc3ac0b2927
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07622480B2

反応ノート

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