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Sodium Hydroxide → HCID 23121981、化合物

HRID 1713503
ノート
印刷プレビュー

反応式

HRID 1713503 の反応式
[H-].[Li+].[Al+3].[H-].[H-].[H-].[N:7]1([CH2:13][CH2:14][NH:15][C:16](=O)OC(C)(C)C)[CH2:12][CH:11]=[CH:10][CH2:9][CH2:8]1.[OH-].[Na+]>O1CCCC1>[N:7]1([CH2:13][CH2:14][NH:15][CH3:16])[CH2:8][CH:9]=[CH:10][CH2:11][CH2:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 23121940HCID 23121940、化合物

生成物 1

HCID 23121981HCID 23121981、化合物収率 42.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

80% Aluminum lithium hydride (0.36 g, 7.5 mmol) was suspended in tetrahydrofuran (10 mL). A solution of 1,1-dimethylethyl N-[2-(3,6-dihydropyridin-1(2H)-yl)ethyl]carbamate (0.68 g, 3.0 mmol) in tetrahydrofuran (10 mL) was added dropwise thereto at room temperature over 10 minutes, and the mixture was refluxed for 3 hours. The reaction solution was cooled to room temperature, and then a 1 N aqueous sodium hydroxide solution (20 mL) was added portionwise thereto. Insolubles were filtered off through a Celite, and the Celite was washed with tetrahydrofuran. The filtrate was concentrated under reduced pressure, and the residue was purified with amino silica gel column chromatography (hexane:ethyl acetate=19:1 to ethyl acetate) to obtain the title compound (0.18 g, yield 42%).

後処理

  1. temperaturethe mixture was refluxed for 3 hours
  2. filtrationInsolubles were filtered off through a Celite
  3. washthe Celite was washed with tetrahydrofuran
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe residue was purified with amino silica gel column chromatography (hexane:ethyl acetate=19:1 to ethyl acetate)

出典と根拠

ORDレコード
ord-5c039b7780d14a95beb719eb36551ce1
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795267B2

反応ノート

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