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2,6-Lutidine → tert-Butyldimethylsilyloxy-1-phenyl-prop-1-yne
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Lutidine | HCID 7937 | — |
| 反応物 | alpha-Ethynylbenzenemethanol | HCID 20155 | — |
| 反応物 | tert-Butyldimethylsilyl trifluoromethanesulphonate | HCID 123564 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | tert-Butyldimethylsilyloxy-1-phenyl-prop-1-yne | HCID 10610466 | — |
反応手順
1-Phenyl-2-propyn-1-ol (7 g) was dissolved in dichloromethane at 0° C. under nitrogen. 2,6-Lutidine (6.17 ml) was added to the solution followed by dropwise addition of tert-butyldimethylsilyl trifluoromethane sulfonate (12.16 ml); the resulting solution was stirred overnight at room temperature. The dichloromethane was washed with water (2×), brine and dried (MgSO4) and solvent removed in vacuo. The residue was purified on flash silica using 100% petrol moving to 5% ethyl acetate/petrol, to afford the title compound as a yellow oil (10.31 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728695 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-df8b8caa74ee4e36b45ccc97b1be26b5 |
| 出典メモ | uspto-grants-1998_03 |