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Water → HCID 11516277、化合物

HRID 743076
ノート
印刷プレビュー

反応式

HRID 743076 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:19][CH2:18][CH:17]([N:20]=[C:21]([C:28]2[CH:29]=[N:30][CH:31]=[CH:32][C:33]=2[NH2:34])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.[OH-].[Na+]>O1CCCC1>[CH2:7]([N:14]1[CH2:19][CH2:18][CH:17]([NH:20][CH:21]([C:28]2[CH:29]=[N:30][CH:31]=[CH:32][C:33]=2[NH2:34])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 11516226HCID 11516226、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 11516277HCID 11516277、化合物収率 63.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of 0.68 g (17.9 mmol) of lithium aluminum hydride in 100 mL of tetrahydrofuran was added dropwise a solution of 6.65 g (17.9 mmol) of 3-[α-{(1-benzylpiperidin-4-yl)imino}benzyl]-4-aminopyridine in tetrahydrofuran 30 ml under reflux, and the mixture was heated under reflux for 1 hour. After being cooled, the mixture was added sequentially with 0.7 mL of water, 0.7 mL of an aqueous 15% sodium hydroxide solution and 2 mL of water, under ice-cooling. After being stirred for 1 hour at ambient temperature, the reaction mixture was filtered through cerite. The filtrate was concentrated and the residue was purified by means of column chromatography (silica gel, 1:9 methanol:chloroform) to give 4.2 g (11.3 mmol) of the title compound.

後処理

  1. temperatureunder reflux
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 1 hour
  4. temperatureAfter being cooled
  5. temperaturecooling
  6. filtrationthe reaction mixture was filtered through cerite
  7. concentrationThe filtrate was concentrated
  8. customthe residue was purified by means of column chromatography (silica gel, 1:9 methanol:chloroform)

出典と根拠

ORDレコード
ord-063b756c294848609f74b86144edd1a4
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05556860

反応ノート

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