反応式
[CH2:1]=[C:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][CH2:3]1.C(OCC)C.[Cl:20][C:21](Cl)([Cl:25])[C:22](Cl)=[O:23].C(=O)(O)[O-].[Na+]>C(COC)OC.[Cu].[Zn]>[Cl:20][C:21]1([Cl:25])[C:2]2([CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][CH2:3]2)[CH2:1][C:22]1=[O:23]参加物
実験手順
49.3 g of tert-butyl 4-methylene-1-piperidine carboxylate was added to a mixture of 157.2 g zinc-copper alloy and 500 ml diethyl ether, and 900 ml solution of 181.8 g trichloroacetyl chloride in dimethoxyethane was added dropwise thereinto over 5.5 hours. After stirred for 30 min, the reaction solution was cooled and saturated aqueous sodium bicarbonate was added thereto at 0° C. or less. The mixture was filtered through Celite and evaporated. The resulting residue was extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated, and the resulting residue was subjected to silica gel column chromatography to give 62.5 g of tert-butyl 1,1-dichloro-2-oxo-7-azaspiro[3.5]nonane-7-carboxylate.
後処理
- temperaturethe reaction solution was cooled
- customat 0° C. or less
- filtrationThe mixture was filtered through Celite
- customevaporated
- extractionThe resulting residue was extracted with ethyl acetate
- washThe extract was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customThe filtrate was evaporated
出典と根拠
- ORDレコード
- ord-73ed4dc326104f7ea5c9ada7ea8b7d5c
- 出典データセット
- uspto-grants-2002_12
- 特許番号
- US06498159B1
関連ノート
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