関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | P,P-Diphenylphosphinodithioic acid | HCID 129564 | — |
| 反応物 | HCID 67179938 | HCID 67179938 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Amino-3-[4-(1,1-difluoroethyl)-phenyl]thioacrylamide | HCID 86632653 | 67.2% |
反応手順
Add diphenylphosphinodithioic acid (13.2 g, 52.9 mmol) to a solution of 3-amino-3-[4-(1,1-difluoroethyl)phenyl]acrylonitrile (5.50 g, 26.4 mmol) in propan-2-ol (264 mL). Heat to 45° C. for 4 h. Dilute with EtOAc (400 mL), wash with brine 3× (100 mL), and evaporate. Crystallize from EtOAc/hexane to afford 3-amino-3-[4-(1,1-difluoroethyl)-phenyl]thioacrylamide. Yield: 67.2%. ES-MS: m/e 243.0 (m+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07960419B2 |
|---|
| 出典データセット | uspto-grants-2011_06 |
|---|
| ORD ID | ord-18afdd9e68fe46b7982c1a289e3bf835 |
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| 出典メモ | uspto-grants-2011_06 |
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