関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydrosulfide hydrate | HCID 16211346 | — |
| 反応物 | 4-bromomethyl-1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazole | HCID 17862868 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | (1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazol-4-yl)-methanethiol | HCID 17862846 | 87% |
反応手順
43.5 g (136.1 mmoles) of 4-bromomethyl-1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazole was added to 300 ml of a N,N-dimethylformamide solution containing 21.8 g (272.2 mmoles) of sodium hydrosulfide hydrate (purity: 70%). The mixture was stirred at room temperature overnight to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into ice water and extraction with diethyl ether was conducted. The resulting organic layer was washed with an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to reduced pressure distillation to remove the solvent contained therein, to obtain 32.3 g (yield: 87.0%) of (1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazol-4-yl)-metha-nethiol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07875606B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-0139c3b7b01d469282f5458362306b2c |
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| 出典メモ | uspto-grants-2011_01 |
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