Hydrogen Peroxide → Tert-butyl 3-oxo-2-oxa-8-azaspiro[4.5]decane-8-carboxylate

HRID 2300178

반응식

HRID 2300178 반응식
[O:1]=[C:2]1[CH2:5][C:4]2([CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]2)[CH2:3]1.OO.[OH-].[Na+].O.O.O.O.O.S([O-])([O-])(=[O:29])=S.[Na+].[Na+]>CO.O.C(OCC)(=O)C>[O:29]=[C:2]1[CH2:3][C:4]2([CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]2)[CH2:5][O:1]1

참가 물질

8

반응물 4

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 61475Sodium Thiosulfate PentahydrateHCID 11195798Tert-butyl 2-oxo-7-azaspiro[3.5]nonane-7-carboxylate

생성물 1

HCID 22744536Tert-butyl 3-oxo-2-oxa-8-azaspiro[4.5]decane-8-carboxylate

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

567 ml solution of 37.8 g tert-butyl 2-oxo-7-azaspiro[3.5]nonane-7-carboxylate in methanol was cooled on ice water, and 43 g of 30% aqueous hydrogen peroxide was added dropwise thereinto. 63 ml of 1 N aqueous sodium hydroxide was added dropwise thereto, and the mixture was stirred at room temperature for 2 hr. 1000 ml ethyl acetate, 600 ml water and 100 ml saturated aqueous sodium thiosulfate pentahydrate were added thereto, and the organic layer was recovered. The extracted solution was washed with brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was evaporated to give 28.4 g of tert-butyl 3-oxo-2-oxa-8-azaspiro[4.5]decane-8-carboxylate.

후처리

  1. additionwas added dropwise
  2. customthe organic layer was recovered
  3. washThe extracted solution was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customThe filtrate was evaporated

출처 및 근거

ORD 기록
ord-9c29fa327797484b8840f6e8c2c0be30
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06498159B1

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