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3-Chloroaniline → 3-((3-Chlorophenyl)amino)-2-cyano-3-(methylthio)acrylamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Chloroaniline | HCID 7932 | — |
| 反応物 | 2-Cyano-3,3-bis(methylthio)acrylamide | HCID 2747746 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-((3-Chlorophenyl)amino)-2-cyano-3-(methylthio)acrylamide | HCID 86698955 | 57% |
反応手順
Dissolved 7.00 g (2-cyano-3,3-bis(methylthio)acrylamide) in 125 mL of ethanol. Then added 4.348 mL (1.10 eq.) of 3-chloroaniline to the reaction vessel and stirred the reaction at 75° C. until starting amide was absent and confirmed by HPLC. Once complete (18 hrs), the reaction was brought to room temperature and filtered to obtain 3-((3-chlorophenyl)amino)-2-cyano-3-(methylthio)acrylamide as an off white to light yellow powder. Product was allowed to dry under vacuum for 1 hr (6.0 g, 57% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09346792B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-13c5edb632ed4d19a0e351cf17c50515 |
| 出典メモ | uspto-grants-2016_05 |