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Methyl isothiocyanate → 1-Methyl-3-trifluoromethanesulphonylthiourea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl isothiocyanate | HCID 11167 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Trifluoromethylsulfonamide | HCID 79001 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Methyl-3-trifluoromethanesulphonylthiourea | HCID 21298882 | 42.3% |
反応手順
A solution of methylisothiocyanate (0.21 g.) in acetone (10 ml.) was added to a solution of trifluoromethanesulphonamide (0.45 g.) and sodium hydroxide (0.12 g.) in water (5 ml.), the mixture stirred at 60° for 18 hours and then evaporated to dryness. The residue was dissolved in water and the solution washed with ethyl acetate and then adjusted to pH 1 with concentrated hydrochloric acid. The mixture was treated with charcoal and filtered and the filtrate extracted with ethyl acetate. The combined ethyl acetate extracts were dried and evaporated to dryness and the residue recrystallized from petroleum ether (b.p. 60°-80°) to give 1-methyl-3-trifluoromethanesulphonylthiourea (0.27 g.), m.p. 88°-90°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04762932 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-fc4168b320ef4c72aa266708c2dd8f0a |
| 出典メモ | uspto-grants-1988_08 |