反応式
[CH3:1][C:2]([OH:16])([C@H:4]([CH3:15])[CH2:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])=[O:7])[CH3:3].[CH3:17][Si:18]([CH3:25])([CH3:24])N1C=CN=C1>CN(C)C=O>[CH3:17][Si:18]([CH3:25])([CH3:24])[O:16][C:2]([CH3:1])([CH3:3])[C@H:4]([CH3:15])[CH2:5][S:6]([C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)(=[O:8])=[O:7]参加物
4
反応条件
- 温度
- 80 °C
実験手順
The compound of Example 10B (0.95 g, 3.9 mmol) was dissolved in 3 mL of dimethylformamide; 1 mL of 1-(trimethylsilyl)imidazole was added, and the resultant solution was stirred overnight at ambient temperature, then heated at 80° C. for 8 hours. The crude mixture was partitioned between ethyl acetate and water; the organic phase was washed with brine and dried over Na2SO4. The solvents were removed in vacuo, and the residue was purified by chromatography on an Analogix Intelliflash 280™, eluting with a gradient of 0% to 20% ethyl acetate in hexanes to provide the titled compound (1.18 g, 96%).
後処理
- customThe crude mixture was partitioned between ethyl acetate and water
- washthe organic phase was washed with brine
- dry with materialdried over Na2SO4
- customThe solvents were removed in vacuo
- customthe residue was purified by chromatography on an Analogix Intelliflash 280™
- washeluting with a gradient of 0% to 20% ethyl acetate in hexanes
出典と根拠
- ORDレコード
- ord-8baa344f47184079aa6489b993392493
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08377913B2
関連ノート
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