Sodium Sulfate → 3-Amino-8-t-butyl-1-oxaspiro(4,5)-decane

HRID 232555ノート

反応式

HRID 232555 の反応式
[C:1]([CH:5]1[CH2:16][CH2:15][C:8]2([O:12][CH2:11][C:10](=[N:13]O)[CH2:9]2)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[NH2:13][CH:10]1[CH2:9][C:8]2([CH2:7][CH2:6][CH:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[CH2:16][CH2:15]2)[O:12][CH2:11]1

参加物

5

反応物 3

HCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydride2 回HCID 867501198-t-Butyl-1-oxaspiro(4,5)decane-3-one oxime

生成物 1

HCID 190401633-Amino-8-t-butyl-1-oxaspiro(4,5)-decane収率 76.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

8-t-Butyl-1-oxaspiro(4,5)-decane-3-one oxime (17.5 g, 76 mmol) in tetrahydrofuran (50 ml) was added to a solution of lithium- aluminium hydride (4.5 g, 0.125 mol) in tetrahydrofuran (100 ml). The reaction mixture was refluxed for 4 hours, cooled end excess LAH was hydrolysed by addition of saturated aqueous sodium sulfate. solids were filtered off washed with tetrahydrofuran and the solvent was stripped off in vacuo. Kugelrohr distillation of the resulting pale yellow oil (16.9 g) gave a colourless oil (12.3 g) Bp.: 125° C./0.02 mbar, nD22 :1.4840.

後処理

  1. temperatureThe reaction mixture was refluxed for 4 hours
  2. filtrationsolids were filtered off
  3. washwashed with tetrahydrofuran
  4. distillationKugelrohr distillation of the resulting pale yellow oil (16.9 g)

出典と根拠

ORDレコード
ord-913d502fa58b48bdb6c8b03c29b3ab54
出典データセット
uspto-grants-1997_01
特許番号
US05591741

反応ノート

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