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Thiophenol → 1-Dimethylamino-3-phenyl-3-phenylthio-2-propene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophenol | HCID 7969 | — |
| 反応物 | 3-(Dimethylamino)-1-phenyl-2-propen-1-one | HCID 353460 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 溶媒 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | 1-Dimethylamino-3-phenyl-3-phenylthio-2-propene | HCID 54193170 | — |
反応手順
By using a method similar to that described in Example 35, but starting from 3-dimethylaminoacrylophenone (80 g), phosphorus oxychloride (40 cc), thiophenol (50.3 cc) and sodium cyanoborohydride (16 g), and crystallising the (Z)-isomer, a yellow solid is isolated after evaporation of the mother liquors under reduced pressure (2.7 kPa) at 30° C. followed by crystallisation of the residue obtained from a mixture of acetone and ethyl ether (25/75 by volume); the solid is recrystallised from methyl ethyl ketone (230 cc). 1-Dimethylamino-3-phenyl-3-phenylthio-2-propene (E) hydrochloride (14.3 g) is thus obtained in the form of a white solid melting at 146°-147° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04755599 |
| 出典データセット | uspto-grants-1988_07 |
| ORD ID | ord-5f17f24339934a9d89f744c2037afce9 |
| 出典メモ | uspto-grants-1988_07 |