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Dimethylformamide → 4,5-dichloro-2-(2,3-dichloro-2-propenyl)-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 | 1,2,3-Trichloro-1-propene | HCID 7286 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4,5-Dichloro-3-hydroxypyridazine | HCID 73247 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4,5-dichloro-2-(2,3-dichloro-2-propenyl)-3(2H)-pyridazinone | HCID 54123359 | 33.5% |
反応手順
To a mixture of 10.8 g of 4,5-dichloro-3(2H)-pyridazinone and 9.5 g of anhydrous potassium carbonate were added 65 ml of N,N-dimethylformamide and stirred for 10 minutes at room temperature. Then, 10.0 g of 1,2,3-trichloro-1-propene (mixture of E-from and Z-form) were added to the mixture solution and were stirred for 6 hours at 40° C. The solution was poured into a large quantity of water and extracted with benzene, and freed of solvent by distillation under reduced pressure to give 6.0 g of the intended compound (mixture of E-form and Z-form). The compound thus obtained was separated into isomer (m.p.: 93.7°-94.6° C., 112.8°-114.8° C.) by means of column chromatography (on silica gel, eluting with benzene).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04945091 |
| 出典データセット | uspto-grants-1990_07 |
| ORD ID | ord-37d2610ee48648fcb89c2630c3c8ed70 |
| 出典メモ | uspto-grants-1990_07 |