反応式
[CH2:1]([N:8]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[OH:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(C)([O-])C.[K+].[C:23]([NH:27][C:28](=[O:31])[CH:29]=[CH2:30])([CH3:26])([CH3:25])[CH3:24]>O1CCCC1>[C:23]([NH:27][C:28](=[O:31])[CH2:29][CH2:30][O:9][N:8]([CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)([CH3:26])([CH3:25])[CH3:24]参加物
5
実験手順
A solution of 21.33 g of dibenzylhydroxylamine in 100 ml of dry tetrahydrofuran is admixed with 1.12 g of potassium-tert-butoxide followed by 12.70 g of N-tert-butylacrylamide. The solution is heated under reflux for 24 hours under N2. The crude reaction mixture is concentrated under reduced pressure and the residue is partitioned between water and methylene chloride. The organic layer is washed with water, brine dried (MgSO4) and evaporated under reduced pressure. Purification by liquid chromatography affords the title compound as an oil.
後処理
- temperatureThe solution is heated
- temperatureunder reflux for 24 hours under N2
- customThe crude reaction mixture
- concentrationis concentrated under reduced pressure
- customthe residue is partitioned between water and methylene chloride
- washThe organic layer is washed with water, brine
- dry with materialdried (MgSO4)
- customevaporated under reduced pressure
- customPurification by liquid chromatography
出典と根拠
- ORDレコード
- ord-93ff27e0422a4cc28e2a15a9a0978d7d
- 出典データセット
- uspto-grants-1991_10
- 特許番号
- US05057563
関連ノート
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