関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-(Phenylmethyl)pyridine | HCID 7581 | — |
| 反応物 | Methyl isothiocyanate | HCID 11167 | — |
| 反応物 | HCID 178506676 | HCID 178506676 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Benzene ether | HCID 22174802 | — |
| 生成物 | N-methyl-2-phenyl-2-(2-pyridyl)thioacetamide | HCID 21539487 | — |
反応手順
2-Benzylpyridine (6.1 g.) dissolved in 25 ml. of dry benzene is added dropwise to 20 ml. of 2M phenyl lithium in benzene/ether with cooling. The mixture is stirred for 30 minutes, then 2.6 g. of methyl isothiocyanate, dissolved in 40 ml. of dry benzene, is added dropwise with cooling. The resulting solution is stirred overnight. An equal volume of water is added and the solution is cooled and made acidic with 10% aqueous hydrochloric acid. The phases are separated, the organic phase is washed with water and the combined aqueous phases are made basic to about pH 9, then extracted with chloroform. The chloroform extracts are washed with water and dried over magnesium sulfate. Filtration and removal of solvent gives a residue which is recrystallized from isopropyl ether/ethanol to give N-methyl-2-phenyl-2-(2-pyridyl)thioacetamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03956325 |
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| 出典データセット | uspto-grants-1976_05 |
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| ORD ID | ord-84de248a71224eaf90692c3ff738b655 |
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| 出典メモ | uspto-grants-1976_05 |
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