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Hydrochloric Acid → 3,3-Bis(2,4-bis(dimethylamino)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-(2,4-Bis(dimethylamino)benzoyl)benzoic acid | HCID 20287212 | — |
| 生成物 | 3,3-Bis(2,4-bis(dimethylamino)phenyl)phthalide | HCID 20216579 | — |
反応手順
A mixture of crude 2-(2,4-bis(dimethylamino)benzoyl)benzoic acid (7 g.), N,N,N',N'-tetramethyl-m-phenylenediamine (1.64 g.) and acetic anhydride was warmed (at 25°-35° C.) during two to three hours, then poured into dilute hydrochloric acid (10%). The resulting mixture was basified and filtered with a filter aid. The filter cake was extracted with hot toluene. Dilution of the toluene extract with hexane afforded 3,3-bis(2,4-bis(dimethylamino)phenyl)phthalide (I: X=Y2 =Y4 =(CH3)2N, Z4 =Z5 =Z6 =Z7 =H) (m.p. 186°-188° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04220357 |
| 出典データセット | uspto-grants-1980_09 |
| ORD ID | ord-26a60b8ba57e4627874ea4144aa19bfb |
| 出典メモ | uspto-grants-1980_09 |