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Water → 6-Chloro-5-fluoro-2-oxo-1-indolinecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chlorosulfonyl isocyanate | HCID 70918 | — |
| 反応物 | 6-Chloro-5-fluoroindolin-2-one | HCID 9794083 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-Chloro-5-fluoro-2-oxo-1-indolinecarboxamide | HCID 13647640 | 10.1% |
反応手順
To a slurry of 6-chloro-5-fluoro-2-oxindole (0.04 mole) in acetonitrile (80 ml) was added chlorosulfonyl isocyanate (6.65 g, 0.047 mole) and the mixture was stirred for 45 minutes. Water (100 ml) was then added and the aqueous mixture was stirred for one hour. The precipitate which formed was filtered off and recrystallized from acetonitrile to give 0.92 g of the title product. Extraction of the filtrate from the aqueous reaction mixture with ethyl acetate (300 ml) followed by drying the extract over MgSO4 and then evaporating it under reduced pressure gave additional product. Recrystallization from acetonitrile gave an additional 2.2 g of product, m.p. 229°-231° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05298522 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-c88dea8392d84c72ba162669590206a9 |
| 出典メモ | uspto-grants-1994_03 |