関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzophenone | HCID 3102 | — |
| 反応物 | 1,5-Dimethyltetrazole | HCID 78825 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2(1-Methyltetrazol-5-yl)-1,1-diphenylethanol | HCID 14724036 | 22% |
反応手順
A solution of 1,5-dimethyltetrazole (20 g; 0.204 mole) in dry THF (200 mL) was cooled to -78° C. and treated with n-butyllithium (91 mL of 2.5 molar solution in hexane; 0.227 mole) and the mixture stirred at -78° C. for 30 minutes. Benzophenone (31.1 g; 0.171 mole) was added and the mixture stirred at -78° C. for 30 minutes and allowed to warm up to 23° C. and stirred for 15 hours. The mixture was quenched with 2N HCl (100 mL) and extracted with EtOAc (3×150 mL). The combined organic layers were dried (MgSO4) and evaporated. The residue was crystallized from EtOAc-Hexane to afford the title compound as a white solid (10.5 g; 22%); m.p.=175°-176° C. (crystallized from EtOAc-hexane). MS (CI): m/e=281 for (M+H)+ ;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04897490 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-3884a5a71c084908aa2492a1684d494f |
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| 出典メモ | uspto-grants-1990_01 |
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