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

HRID 47342

反応式

HRID 47342 の反応式
[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

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a505a4a908504f4f8d513ef2b414c003
出典データセット
uspto-grants-2004_03
特許番号
US06699870B2

関連ノート

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