Ethyl Acetate → HCID 73656239、化合物

HRID 1885737ノート

反応式

HRID 1885737 の反応式
[Cl:1][C:2]1[CH2:3][N:4]=[CH:5][C:6]2([CH3:21])[CH:17]([CH3:18])[CH:15]3[CH2:16][C:10]4=[C:11]([N:14]3C#N)[CH2:12][CH2:13][C:7]2=[C:8]4[CH:9]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)(=O)C.[OH-].[Na+]>O1CCCC1.O>[Cl:1][C:2]1[CH2:3][N:4]=[CH:5][C:6]2([CH3:21])[CH:17]([CH3:18])[CH:15]3[CH2:16][C:10]4=[C:11]([NH:14]3)[CH2:12][CH2:13][C:7]2=[C:8]4[CH:9]=1

参加物

7

反応物 4

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 53643109HCID 53643109、化合物

生成物 1

HCID 73656239HCID 73656239、化合物収率 18%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

The nitrile (6.41 g) was dissolved in 300 ml of tetrahydrofuran and, 4.06 g lithium aluminum hydride was added, with stirring. The suspension was heated at reflux for 2 hr and ethyl acetate, water, aqueous sodium hydroxide solution and water were added. The suspension was filtered and the filtrate was concentrated. The residue was triturated with ether and the solid was recrystallized from methanol to give 0.64 g (18%) of the product, mp 260°-263° C. (dec.).

後処理

  1. temperatureThe suspension was heated
  2. temperatureat reflux for 2 hr
  3. filtrationThe suspension was filtered
  4. concentrationthe filtrate was concentrated
  5. customThe residue was triturated with ether
  6. customthe solid was recrystallized from methanol

出典と根拠

ORDレコード
ord-f0157005e31b47d5a5df5ad1ffb1ea49
出典データセット
uspto-grants-1992_09
特許番号
US05145965

反応ノート

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