関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (Trimethylsilyl)imidazole | HCID 28925 | — |
| 反応物 | (3s)-2,3-Dimethyl-4-(phenylsulfonyl)butan-2-ol | HCID 13964863 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Trimethyl{[(2s)-1,1,2-trimethyl-3-(phenylsulfonyl)propyl]oxy}silane | HCID 68938726 | 96% |
反応手順
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%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08377913B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-8baa344f47184079aa6489b993392493 |
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| 出典メモ | uspto-grants-2013_02 |
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