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Hydrochloric Acid → 3-(2,4-Bis(dimethylamino)phenyl)-3-(2-ethoxy-4-(diethylamino)phenyl)phthalide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 1,3-Benzenediamine, N1,N1,N3,N3-tetramethyl- | HCID 89715 | — |
| 反応物 | 2-[4-(Diethylamino)-2-ethoxybenzoyl]benzoic acid | HCID 15519332 | — |
| 生成物 | 3-(2,4-Bis(dimethylamino)phenyl)-3-(2-ethoxy-4-(diethylamino)phenyl)phthalide | HCID 23343363 | — |
反応手順
A mixture of 2-(2-ethoxy-4-(diethylamino)benzoyl)-benzoic acid (6.82 g.), N,N,N',N'-tetramethyl-m-phenylenediamine (2.80 g.) and acetic anhydride (20 g.) was heated (70°-75° C.) during one hour, let stand overnight and poured into dilute hydrochloric acid. The resulting mixture was basified. Recrystallization of the resulting red precipitate from hexane followed by slurrying in alkaline water afforded 3-(2,4-bis(dimethylamino)phenyl)-3-(2-ethoxy-4 -(diethylamino)phenyl)phthalide (I: X= (CH3)2N, Y2 = CH3CH2O, Y4 = (CH3CH2)2N, Z4 = Z5 = Z6 = Z7 = H) (m.p. 146°-150° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04032527 |
| 出典データセット | uspto-grants-1977_06 |
| ORD ID | ord-ad08ec883b8845fe93c6b6f90673409b |
| 出典メモ | uspto-grants-1977_06 |