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

HRID 232555노트

반응식

HRID 232555 반응식
[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

참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydride2회HCID 867501198-t-Butyl-1-oxaspiro(4,5)decane-3-one oxime

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-913d502fa58b48bdb6c8b03c29b3ab54
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591741

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