Water → 1344144-96-2

HRID 2276774ノート

反応式

HRID 2276774 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]2([C:13]#[N:14])[CH2:12][CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]2([CH2:13][NH2:14])[CH2:12][CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 67453617HCID 67453617、化合物

生成物 1

HCID 674510161344144-96-2収率 94.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 1-(6-methoxypyridin-2-yl)cyclobutanecarbonitrile (1.7 g, 8.8 mmol) in THF (20 mL) was added lithium aluminum hydride solution (1.0 M in THF, 11 mL, 11 mmol). The mixture was refluxed for 1.5 h and allowed to cool to room temperature. Water (0.43 mL) was slowly added, followed by 0.43 mL of 3 M NaOH, and then three additions of 0.43 mL of water. The resulting mixture was filtered through diatomaceous earth and rinsed with THF. The combined organics were dried over Na2SO4 and concentrated to dryness to give the desired product (1.6 g) as a viscous oil.

後処理

  1. temperatureThe mixture was refluxed for 1.5 h
  2. filtrationThe resulting mixture was filtered through diatomaceous earth
  3. washrinsed with THF
  4. dry with materialThe combined organics were dried over Na2SO4
  5. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-49f2b9dd125a49f788ecd92eb7bce5d3
出典データセット
uspto-grants-2015_09
特許番号
US09133123B2

反応ノート

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