関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1-(m-Tolyl)piperazine dihydrochloride | HCID 83110 | — |
| 反応物 | 3,6-Dibromopyridazine | HCID 248852 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Bromo-6-[4-(3-methylphenyl)-1-piperazinyl]pyridazine | HCID 503326 | 61.5% |
反応手順
A mixture of 5 parts of 1-(3-methylphenyl)piperazine dihydrochloride, 10.6 parts of sodium carbonate and 180 parts of N,N-dimethylformamide was stirred for 1 hour at 65° C. Then there were added 7.2 parts of 3,6-dibromopyridazine and the whole was stirred overnight at about 65° C. The reaction mixture was poured into ice water. The product was filtered off and dissolved in dichloromethane. The solution was washed twice with water, dried, filtered and evaporated. The residue was crystallized from ethanol. The product was filtered off and dried, yielding 4.1 parts (61.5%) of 3-bromo-6-[4-(3-methylphenyl)-1-piperazinyl]pyridazine; mp. 145.7° C. (compound 136).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05157035 |
|---|
| 出典データセット | uspto-grants-1992_10 |
|---|
| ORD ID | ord-4138cb209a69424abe1aa1f8b81038e0 |
|---|
| 出典メモ | uspto-grants-1992_10 |
|---|