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Lawesson's reagent → 2-(tert-Butyl)-5-methyl-1,3,4-thiadiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lawesson's reagent | HCID 87949 | — |
| 反応物 | N'-acetyl-2,2-dimethylpropanohydrazide | HCID 23525705 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(tert-Butyl)-5-methyl-1,3,4-thiadiazole | HCID 22943597 | — |
反応手順
A mixture of the product from Example 50A (158 mg, 1 mmol) and Lawesson's reagent (808 mg, 2 mmol) in tetrahydrofuran (4 mL) was heated at reflux for 2 hours. The solution was concentrated, dissolved in dichloromethane (15 mL) and washed with saturated sodium bicarbonate solution (10 mL). The resulting organic layer was passed through a silica pad and washed with dichloromethane and ethyl acetate (10:1). The solvent was evaporated to provide the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.39 (s, 9 H) 2.67 (s, 3 H); MS (ESI) m/z 157 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08481574B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-f61e161cd16d467b82426c41be70e703 |
| 出典メモ | uspto-grants-2013_07 |