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Cyanogen Bromide → 6-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyanogen Bromide | HCID 10476 | — |
| 反応物 | 3-Chloro-6-hydrazinyl-4,5-dimethylpyridazine | HCID 12648042 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide | HCID 86650797 | 100.2% |
反応手順
(6-Chloro-4,5-dimethylpyridazin-3-yl)hydrazine (W3.006; 12 g) was initially charged in EtOH (240 ml) and water (50 ml) while stirring at RT. Thereafter, cyanogen bromide (14.7 g) in a mixture of EtOH (120 ml) and water (25 ml) was slowly added dropwise at RT. After stirring at RT for 6 h, the mixture was left to stand overnight. Then the mixture was dried and the residue was purified using silica gel (80 g cartridge, DCM/methanol gradient of 0-20% in 60 min). 19.4 g of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09079906B2 |
| 出典データセット | uspto-grants-2015_07 |
| ORD ID | ord-770df7b676fd4cb9b4008a42023db1f0 |
| 出典メモ | uspto-grants-2015_07 |