関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | 6-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide | HCID 86650797 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-Ethoxy-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine | HCID 58046005 | 108.9% |
反応手順
6-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.006; 4 g) were dissolved in ethanol (120 ml), admixed under argon with sodium ethoxide (5.86 g) and stirred at 60° C. for 1 h. Then the mixture was dried and the residue was purified using a 40 g silica gel cartridge (0-20% dichloromethane-ethanol gradient in 40 min). The clean product fractions were combined and dried. 3.24 g of the title compound were obtained, which still contained residual amounts of dichloromethane. LC-MS rt: 0.53 min [M+H]+: 208.1 (met. b)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08076336B2 |
|---|
| 出典データセット | uspto-grants-2011_12 |
|---|
| ORD ID | ord-474fb6ecf36e4e5f8d83674cfebd422c |
|---|
| 出典メモ | uspto-grants-2011_12 |
|---|