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Dimethylformamide → 6-[4-(N-methylthiocarbamoylamino)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Ici 109,081 | HCID 161928 | — |
| 反応物 | Methylthioisocyanate | HCID 21933440 | — |
| 生成物 | 6-[4-(N-methylthiocarbamoylamino)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone | HCID 13217342 | — |
反応手順
In 40 ml of dry dimethylformamide (DMF) was dissolved 8.13 g of 6-(p-aminophenyl)-5-methyl-4,5-dihydro-3(2H)-pyridazinone. To this solution was added 3.5 g of methyl thioisocyanate, and the mixture was stirred for 4 hours at room temperature. The mixture was stirred for an additional 30 minutes at 50° C. and the solvent was distilled off under reduced pressure. To the residue was added 50 ml of dichloromethane/ether (1:1) to precipitate crystals which were then collected by filtration and washed with dichloromethane, whereby 10.1 g of the above-identified compound was obtained. M.P. 213° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04521415 |
| 出典データセット | uspto-grants-1985_06 |
| ORD ID | ord-019e8b913817441084cde6b12912015a |
| 出典メモ | uspto-grants-1985_06 |