Acetic Anhydride → 3-(2,4-Bis(dimethylamino)phenyl)-3-(4-(diethylamino)phenyl)-4,5,6,7-tetrachlorophthalide

関与物質

役割	名称	HCID	仕込み量
反応物	Acetic Anhydride	HCID 7918	—
反応物	1,3-Benzenediamine, N1,N1,N3,N3-tetramethyl-	HCID 89715	—
反応物	3,4,5,6-Tetrachloro-2-carboxy-4'-diethylaminobenzophenone	HCID 19956611	—
溶媒	Methanol	HCID 887	—
生成物	3-(2,4-Bis(dimethylamino)phenyl)-3-(4-(diethylamino)phenyl)-4,5,6,7-tetrachlorophthalide	HCID 53676727	48.2%

反応条件

温度	90 °C

反応手順

A mixture of 2-(4-(diethylamino)benzoyl)-3,4,5,6-tetrachlorobenzoic acid (8.70 g.), N,N,N',N'-tetramethyl-m-phenylenediamine (3.61 g.) and acetic anhydride (5 ml.) was heated (to 90° C.). Addition of methanol (10 ml.) and slurrying the resulting product with methanol afforded 3-(2,4-bis(dimethylamino)phenyl)-3-(4-(diethylamino)phenyl)-4,5,6,7-tetrachlorophthalide (I: X=(CH3)2N, Y2 =H, Y4 =(CH3CH2)2N, Z4 =Z5 =Z6 =Z7 =Cl) (5.60 g., m.p. 206°-207.5° 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-3753fa9fd15a408684a887bf0642641e
出典メモ	uspto-grants-1980_09