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Triethylamine → 6-chloro-1H-imidazo[4,5-c]pyridine-2(3H)-thione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| 反応物 | 6-Chloropyridine-3,4-diamine | HCID 817133 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-chloro-1H-imidazo[4,5-c]pyridine-2(3H)-thione | HCID 90041681 | — |
反応手順
A stirred mixture of 6-chloropyridine-3,4-diamine (500 mg, 3.48 mmol), 1,1′-thiocarbonyldiimidazole (1.24 g, 6.97 mmol), and triethylamine (0.49 mL, 3.48 mmol) in anhydrous DMF (15.0 mL) was microwaved in a Biotage Initiator at 100° C. at normal power for 1 h. Then the reaction mixture was evaporated at reduced pressure, and the resulting residue extracted with DCM (200 mL) and allowed to stand at 10° C. overnight. The mixture filtered and the solids washed with cold DCM (2×20 mL), and air dried to afford the title compound as a solid. LC-MS: calculated for C6H4ClN3S 184.98 observed m/e: 186.07 (M+H)+ (Rt 0.62/2.0 min)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09290517B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-dfb30f55ec3e46d28a7030b19bf08bed |
| 出典メモ | uspto-grants-2016_03 |