化工社化工社 化学情報印刷レポート · 研究参考用
Hexane → 4-(1,3-Dioxolan-2-yl)-5-tributylstannylthiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Tributyltin Chloride | HCID 15096 | — |
| 反応物 | 2-Bromo-4-(1,3-dioxolan-2-yl)thiazole | HCID 21952286 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(1,3-Dioxolan-2-yl)-5-tributylstannylthiazole | HCID 21952069 | 98.1% |
反応手順
2-Bromo-4-(1,3-dioxolan-2-yl) thiazole (6.4 g ,27.14 mmol) was stirred at −78° C. in dry THF (38 ml). 1.6M n butyl lithium in hexane (18.6 ml, 29.78 mmol) was added dropwise under nitrogen. After 30 min at this temperature, tributyl tin chloride (7.35 ml, 27.14 mmol) was added dropwise. The reaction was allowed to warm to 0° and water (20 ml) was added. The product was extracted into ether (3×100 ml). The combined organic extracts were dried (MgSO4 ) and evaporated. The residue was triturated with isohexane (3×100 ml) and the mother liquors were decanted, combined and concentrated to give a brown oil (11.88 g); m/z 444–450.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084147B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-8f9cade0188a4427a37fc2196adc5311 |
| 出典メモ | uspto-grants-2006_08 |