Hydrochloric Acid → 3-(2,4-Bis(dimethylamino)phenyl)-3-(2-ethoxy-4-(diethylamino)phenyl)phthalide

HRID 839539

反応式

HRID 839539 の反応式
[CH2:1]([O:3][C:4]1[CH:20]=[C:19]([N:21]([CH2:24][CH3:25])[CH2:22][CH3:23])[CH:18]=[CH:17][C:5]=1[C:6]([C:8]1[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=1[C:10](O)=[O:11])=[O:7])[CH3:2].[CH3:26][N:27]([CH3:37])[C:28]1[CH:33]=[CH:32][CH:31]=[C:30]([N:34]([CH3:36])[CH3:35])[CH:29]=1.C(OC(=O)C)(=O)C.Cl>>[CH3:35][N:34]([CH3:36])[C:30]1[CH:29]=[C:28]([N:27]([CH3:37])[CH3:26])[CH:33]=[CH:32][C:31]=1[C:6]1([C:5]2[CH:17]=[CH:18][C:19]([N:21]([CH2:22][CH3:23])[CH2:24][CH3:25])=[CH:20][C:4]=2[O:3][CH2:1][CH3:2])[C:8]2[C:9](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:10](=[O:11])[O:7]1

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 897151,3-Benzenediamine, N1,N1,N3,N3-tetramethyl-HCID 155193322-[4-(Diethylamino)-2-ethoxybenzoyl]benzoic acid

生成物 1

HCID 233433633-(2,4-Bis(dimethylamino)phenyl)-3-(2-ethoxy-4-(diethylamino)phenyl)phthalide

実験手順

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 = Z 6 = Z7 = H) (m.p. 146°-150° C.).

後処理

  1. temperaturewas heated (70°-75° C.) during one hour
  2. customRecrystallization of the resulting red precipitate from hexane

出典と根拠

ORDレコード
ord-e6de2efb25294d94961b9e401015c4f2
出典データセット
uspto-grants-1978_06
特許番号
US04096176

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