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Water → 6-Methylthio-2-oxindole-1-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Chlorosulfonyl isocyanate | HCID 70918 | — |
| 反応物 | 6-Methylthiooxindole | HCID 21282070 | — |
| 生成物 | 6-Methylthio-2-oxindole-1-carboxamide | HCID 86740521 | — |
反応手順
Chlorosulfonyl isocyanate (5.66 g, 0.04 mole) was added to a slurry of 6-methylthio-2-oxindole (6.0 g, 0.033 mole) in acetonitrile (60 ml) at 5° to 10° C. The reaction mixture was stirred for one hour. Water (100 ml) was then added to said mixture with good stirring for ten minutes. The aqueous solution was extracted with ethyl acetate (600 ml), washed successively with water and brine, dried (MgSO4) and evaporated under reduced pressure to give a gray solid which was recrystallized from acetonitrile Yield=3.0 g. An additional 0.71 g of product was obtained from the mother liquor. Total yield=3.71 g (50.6%); m.p. 176°-179° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04665194 |
| 出典データセット | uspto-grants-1987_05 |
| ORD ID | ord-0fa7d40d21194116a1601424b07ca8fb |
| 出典メモ | uspto-grants-1987_05 |