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Cyclobutanecarbonyl chloride → N-(3-(3-methyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)cyclobutanecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyclobutanecarbonyl chloride | HCID 78705 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-Methyl-6-[3-(amino)phenyl]-1,2,4-triazolo[4,3-b]pyridazine | HCID 12726868 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(3-(3-methyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)cyclobutanecarboxamide | HCID 15595670 | 25.7% |
反応手順
To a solution of 7.0 g of 3-methyl-6-(3-aminophenyl)-1,2,4-triazolo[4,3-b]pyridazine in 1.5 liters of dichloromethane was added 6 ml of N,N-diisopropylethylamine and 4.0 g of cyclobutane carboxylic acid chloride. This soltution was stirred for 4 hours, washed with 200 ml of saturated aqueous sodium bicarbonate, dried and evaported in vacuo. A small amount of dichloromethane was added and the mixture warmed to give 2.45 g of crystals. A second crop (3.5 g) was recovered from the mother liquor. Recrystallization from dichloromethane-hexane gave the desired compound as white crystals, mp 242°-245° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04767765 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-d292970282fe4c22ab595e474606dacb |
| 出典メモ | uspto-grants-1988_08 |