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Hydrochloric Acid → 4-(tert-Butyl)-3-chloro-6-hydrazinylpyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 4-tert-Butyl-3,6-dichloropyridazine | HCID 89846 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(tert-Butyl)-3-chloro-6-hydrazinylpyridazine | HCID 22987886 | 61.3% |
反応手順
To a solution of 3,6-dichloro-4-(1,1-dimethylethyl)pyridazine (2.0 g, 9.76 mmol) in ethanol (30 ml) was added hydrazine hydrate (0.34 ml, 10.9 mmol) dropwise. The reaction mixture was heated at reflux for 18 h under an atmosphere of nitrogen. The solvent was removed under high vacuum to leave a residue to which was added 5N hydrochloric acid (50 ml). The solution obtained was washed with dichloromethane (20 ml) and the aqueous layer was poured on to a mixture of ice and aqueous ammonia. The resultant solid was collected by filtration and dried under vacuum to yield the title compound (1.2 g). Data for the title compound: 1H NMR (360 MHz, DMSO) δ1.39 (3H, t, J=7.3 Hz), 4.35 (2H), 7.07 (1H, s), 8.07 (1H, s); MS (ES+) m/e 201, 203 [MH]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06500828B1 |
| 出典データセット | uspto-grants-2002_12 |
| ORD ID | ord-2e2d0de0385d4b068fccc0379568d93a |
| 出典メモ | uspto-grants-2002_12 |