化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → 1-Phenyltriazolylmethyl-3-hydroxypyridine-2-thione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Boron tribromide | HCID 25134 | — |
| 反応物 | 1-Phenyltriazolylmethyl-3-methoxypyridine-2-thione | HCID 178487643 | — |
| 生成物 | 1-Phenyltriazolylmethyl-3-hydroxypyridine-2-thione | HCID 178515729 | 67.3% |
反応手順
Reaction of 153a (0.28 g, 0.93 mmol) and 1M BBr3 in CH2Cl2 (1.5 equiv) within 48 h as described for the synthesis of 148a gave compound 154a (0.178 g, 67%) as olive green solid. 1H NMR (400 MHz, CDCl3) δ 8.43 (d, J=16.6 Hz, 1H), 8.39 (s, 1H), 7.79 (dd, J=6.6, 1.3 Hz, 1H), 7.69 (m, 2H), 7.46 (m, 3H), 6.97 (dd, J=7.7, 1.2 Hz, 1H), 6.69 (dd, J=7.6, 6.8 Hz, 1H), 5.94 (s, 2H). 13C NMR (100 MHz, CDC3) δ 168.59, 155.12, 141.60, 136.66, 131.65, 129.69, 128.99, 122.57, 120.60, 114.04, 112.47, 77.30, 76.99, 76.67, 52.08. HRMS (EI) calcd for C14H12N4OS [M]+ 284.0730. found 284.0732.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871728B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-a4d8c3f230314695992f9ea23d163ebf |
| 出典メモ | uspto-grants-2014_10 |