(Trimethylsilyl)imidazole → Trimethyl{[(2s)-1,1,2-trimethyl-3-(phenylsulfonyl)propyl]oxy}silane
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%).