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Water → ethyl 2-(4-chloro-2-fluoro-5-(-methylethoxy)phenylaminothioxometyl)-3,4,5,6-tetrahydro1(2H)pyridazinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1(2H)-Pyridazinecarboxylic acid, tetrahydro-, ethyl ester | HCID 3014377 | — |
| 反応物 | 1-Chloro-5-fluoro-4-isothiocyanato-2-[(propan-2-yl)oxy]benzene | HCID 13607933 | — |
| 触媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | ethyl 2-(4-chloro-2-fluoro-5-(-methylethoxy)phenylaminothioxometyl)-3,4,5,6-tetrahydro1(2H)pyridazinecarboxylate | HCID 15590227 | — |
反応手順
4-Chloro-2-fluoro-5-(1-methylethoxy)phenyl isothiocyanate (2.8 g) was added to a solution of 2-ethoxycarbonyl-3,4,5,6-tetrahydro-(1H,2H)-pyridazine (1.8 g) and several drops of triethylamine in toluene (5 ml), and the resultant mixture was stirred at 25° C. overnight. Water was added to the mixture, which was then extracted with toluene. The toluene layer was washed with water, dried and concentrated.The residue was purified by silica gel column chromatography to give 2 of ethyl 2-(4-chloro-2fluoro-5-(1-methylethoxy)phenylaminothioxomethyl)-3,4,5,6-tetrahydro-1(2H) pyridazine carboxylate. nD27.5 1.5534. NMR δ (ppm): 1.3 (3H, t), 1.4 (6H, d), 1.8 (4H, m), 4.35 (2H, q), 7.1 (1H, d), 8.0 (1H, d), ##STR12##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04452981 |
| 出典データセット | uspto-grants-1984_06 |
| ORD ID | ord-4fbc14257b414844941e63c4614ea337 |
| 出典メモ | uspto-grants-1984_06 |