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Hydrogen Sulfide → Thiobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Sulfide | HCID 402 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3,5-Bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzonitrile | HCID 10041643 | — |
| 生成物 | Thiobenzamide | HCID 683563 | — |
反応手順
Into a solution containing 10.0 g (0.03 mole) of 3,5-bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzonitrile, 5.7 ml (0.04 mole) of triethylamine and 14.2 ml (0.18 mole) of pyridine, hydrogen sulfide gas is bubbled over 15 hours. The mixture is poured into ice water (110 ml), and an oily precipitate solidifies upon standing at 0° C. for 15 hours. The solid is thoroughly washed with water and filtered. Recrystallization from ethyl acetate and hexane gives 7.9 g (71%) of analytically pure 3,5-bis(1,1-dimethylethyl)-4-[2-methoxyethoxy)methoxy]benzenecarbothioamide, mp 113°-115° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05376670 |
| 出典データセット | uspto-grants-1994_12 |
| ORD ID | ord-7a3dd12f1bb742cc82f4c31fdaf3cc22 |
| 出典メモ | uspto-grants-1994_12 |