Lithium Hydroxide → 4-(5-Nitropyridin-2-yl)butanenitrile

HRID 1504964ノート

反応式

HRID 1504964 の反応式
[C:1]([CH2:3][CH2:4][C:5]([C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][N:15]=1)(C(OC)=O)C(OC)=O)#[N:2].[Li+].[OH-]>CO.O>[N+:20]([C:17]1[CH:18]=[CH:19][C:14]([CH2:5][CH2:4][CH2:3][C:1]#[N:2])=[N:15][CH:16]=1)([O-:22])=[O:21]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 68292301HCID 68292301、化合物

生成物 1

HCID 682920074-(5-Nitropyridin-2-yl)butanenitrile収率 95%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of compound 76 (3.3 g, 10.7 mmol) in CH3OH (100 mL) was added a solution of LiOH (15.4 g, 64.2 mmol) in H2O (100 mL) at room temperature with stirring. The mixture was stirred at room temperature for 2 h. Methanol was removed in vacuo and the residual aqueous solution was washed with EtOAc (two times), then was acidified to pH=2 with 1N HCl. The aqueous phase was extracted with EtOAc. The combined organic extract was dried over Na2SO4, then was stirred at 50° C. for overnight. The solution was concentrated to afford compound 77 (1.9 g, 95%) as a yellow oil.

後処理

  1. stirringThe mixture was stirred at room temperature for 2 h
  2. customMethanol was removed in vacuo
  3. washthe residual aqueous solution was washed with EtOAc (two times)
  4. extractionThe aqueous phase was extracted with EtOAc
  5. extractionThe combined organic extract
  6. dry with materialwas dried over Na2SO4
  7. stirringwas stirred at 50° C. for overnight
  8. concentrationThe solution was concentrated

出典と根拠

ORDレコード
ord-c09be9ae0b944f12b24d89018c9765c8
出典データセット
uspto-grants-2015_12
特許番号
US09216957B2

反応ノート

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