関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl isovalerate | HCID 7945 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triisopropylsilyl trifluoromethanesulfonate | HCID 2724529 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 溶媒 | 2(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl- | HCID 81646 | — |
| 生成物 | (1-Ethoxy-3-methyl-but-1-enyloxy)-triisopropyl-silane | HCID 53927273 | — |
反応手順
Tetrahydrofuran (100 ml) and 1,3-dimethyl-3,4,5,6-tetrahydro 2 (1H)-pyrimidinone (140 ml) were mixed at -20° C. and lithium bis (trimethylsilyl) amide (1M in tetrahydrofuran, 100 ml) was added. The mixture was cooled to -70° C., ethyl isovalerate (18.75 ml) added and stirred for 1/2 hour at -70° C. Triisopropylsilyl trifluoromethane sulfonate was added and the mixture left to stir at -75° C. for 1/2 hour before warming to room temperature and stirring for 3 hours. The reaction mixture was quenched with aqueous sodium bicarbonate (8%, 150 ml) and extracted with hexane (1000 ml). The hexane extract was washed with water (4×500 ml), dried (MgSO4), filtered and concentrated in vacuo to afford a crude yellow oil containing the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06057457 |
|---|
| 出典データセット | uspto-grants-2000_05 |
|---|
| ORD ID | ord-726b5dc3d5e546078e9063c640fb4a48 |
|---|
| 出典メモ | uspto-grants-2000_05 |
|---|