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Acetic Anhydride → 3-(2,4-Bis(diethylamino)phenyl)-3-(2-methyl-4-(diethylamino)phenyl)phthalide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 2-(4-(Diethylamino)-2-methylbenzoyl)benzoic acid | HCID 104335 | — |
| 反応物 | N~1~,N~1~,N~3~,N~3~-Tetraethylbenzene-1,3-diamine | HCID 19382815 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(2,4-Bis(diethylamino)phenyl)-3-(2-methyl-4-(diethylamino)phenyl)phthalide | HCID 86734898 | — |
反応手順
A mixture of 2-(2-methyl-4-(diethylamino)benzoyl)benzoic acid (12.48 g.), N,N,N',N'-tetraethyl-m-phenylenediamine (10.56 g.) and acetic anhydride (12 ml.) was warmed (at 40°±8° C.) during one hour, diluted with water (50 ml., then 100 ml.), adjusted to pH 4.6 and filtered. The filtrate was clarified with water and adjusted to pH 5.5. Recrystallization of the resulting product (m.p. 134°-140° C.) from methanol afforded 3-(2,4-bis(diethylamino)phenyl)-3-(2-methyl-4-(diethylamino)phenyl)phthalide (I: X=Y4 =(CH3CH2)2N, Y2 =CH3, Z4 =Z5 =Z6 =Z7 =H) (m.p. 149°-151° 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-fa66cc458c26455bb8925a70dd2f5bc7 |
| 出典メモ | uspto-grants-1980_09 |