Dimethylformamide → Butyl 4-oxopiperidine-1-carboxylate
反応式
O.Cl.[NH:3]1[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.C(N([CH2:15][CH3:16])CC)C.[C:17]([O:20][C:21]([O-])=O)([O-])=[O:18].[CH3:24]N(C)C=O>>[CH2:21]([O:20][C:17]([N:3]1[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1)=[O:18])[CH2:24][CH2:15][CH3:16]参加物
5
実験手順
About 2 g of 4-piperidone hydrochloride monohydrate (FIG. 10a) was dissolved in about 30 ml of N,N-dimethylformamide at temperatures of between about 110-115° C. The solution was cooled to room temperature, and to this solution was added about 2.6 g of triethyl amine and a solution containing about 3.06 g of ditertarybutyl dicarbonate in 10 ml DMF. The reaction was continued for about 24 hours at room temperature. The DMF was removed under reduced pressure. About 100 ml of water was added to the residue and the mixture was extracted with ethyl ether (2×100 ml), and the organic layer dried over anhydrous MgSO4. The ether was evaporated to dryness under reduced pressure to yield about 2.33 g of the compound of FIG. 10b.
後処理
- customThe DMF was removed under reduced pressure
- additionAbout 100 ml of water was added to the residue
- extractionthe mixture was extracted with ethyl ether (2×100 ml)
- dry with materialthe organic layer dried over anhydrous MgSO4
- customThe ether was evaporated to dryness under reduced pressure
出典と根拠
- ORDレコード
- ord-f73a84b269f4451bb2a370f803eab873
- 出典データセット
- uspto-grants-2002_07
- 特許番号
- US06420370B1
反応ノート
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