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Sodium Hydroxide → [(4-Chloro-1H-pyrazol-1-yl)oxy]methyl thiocyanate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Thiocyanic acid, chloromethyl ester | HCID 76755 | — |
| 反応物 | Tetrabutylammonium Hydroxide | HCID 2723671 | — |
| 反応物 | 4-Chloro-1H-pyrazol-1-ol | HCID 13391252 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | [(4-Chloro-1H-pyrazol-1-yl)oxy]methyl thiocyanate | HCID 14011041 | 71.6% |
反応手順
50 ml of a 5% strength aqueous sodium hydroxide solution were added to 5 g (42 mMol) of 4-chloro-1-hydroxypyrazole, 13.5 g (126 mMol) of chloromethyl thiocyanate and 50 ml of methylene chloride. After the addition of 1 g (4 mMol) of tetra-n-butylammonium hydroxide, the mixture was stirred at room temperature for 24 hours. Thereafter, the organic phase was separated off, dried and evaporated down. Distillation of the residue under reduced pressure (airbath at 140° C./3 mbar) gave 5.7 g (71% of theory) of 4-chloro-1-[(thiocyanato)-methoxy]-pyrazole (compound No. 1), which was recrystallized from ether/petroleum ether (mp. 60° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04764527 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-e1f2e11ee6ab46f19657e1637b95bd26 |
| 出典メモ | uspto-grants-1988_08 |