Water → HCID 19960978、化合物

HRID 53880ノート

反応式

HRID 53880 の反応式
[CH2:1]([N:8]1[CH2:15][C:14]2([C:16]#[N:17])[CH:10]([CH2:11][O:12][CH2:13]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[NH2:17][CH2:16][C:14]12[CH2:15][N:8]([CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH2:9][CH:10]1[CH2:11][O:12][CH2:13]2

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 19960963HCID 19960963、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 19960978HCID 19960978、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

3.7 g (15.9 mmol) of 7-benzyl-1-cyano-3-oxa-7-azabicyclo[3.3.0]octane in 5 ml of absolute tetrahydrofuran are added dropwise to a mixture of 1.5 g of lithium aluminium hydride in 100 ml of absolute tetrahydrofuran and the resulting mixture is heated under reflux for 15 hours. Decomposition is effected with 1.5 ml each of water, 15% strength sodium hydroxide solution, and again water, and the mixture is filtered with suction, and the aluminium salts are extracted by boiling on two occasions with 100 ml of tetrahydrofuran. The tetrahydrofuran solutions are concentrated and the residue is distilled. Yield: 3.2 g (86% of theory) Boiling point: 125°-130° C./0.04 mbar

後処理

  1. temperaturethe resulting mixture is heated
  2. temperatureunder reflux for 15 hours
  3. filtrationthe mixture is filtered with suction
  4. extractionthe aluminium salts are extracted
  5. concentrationThe tetrahydrofuran solutions are concentrated
  6. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-d37da7198475475b83000f1d89aa6a2d
出典データセット
uspto-grants-1997_04
特許番号
US05621105

反応ノート

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