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

HRID 27008

반응식

HRID 27008 반응식
[CH3:1][N:2]([CH3:20])[C:3]1[CH:19]=[CH:18][C:6]([C:7]([C:9]2[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=2[C:11]([OH:13])=[O:12])=O)=[CH:5][CH:4]=1.[CH3:21][N:22]([CH3:32])[C:23]1[CH:28]=[CH:27][CH:26]=[C:25]([N:29]([CH3:31])[CH3:30])[CH:24]=1.C(OC(=O)C)(=O)C.Cl>>[CH3:30][N:29]([CH3:31])[C:25]1[CH:24]=[C:23]([N:22]([CH3:32])[CH3:21])[CH:28]=[CH:27][C:26]=1[C:7]1([C:6]2[CH:18]=[CH:19][C:3]([N:2]([CH3:20])[CH3:1])=[CH:4][CH:5]=2)[C:9]2[C:10](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:11](=[O:13])[O:12]1

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 889372-[4-(Dimethylamino)benzoyl]benzoic acidHCID 897151,3-Benzenediamine, N1,N1,N3,N3-tetramethyl-

생성물 1

HCID 204408323-(2,4-Bis(dimethylamino)phenyl)-3-(4-(dimethylamino)phenyl)phthalide

반응 조건

온도
95 °C

실험 절차

A mixture of 2-(4-(dimethylamino)benzoyl)benzoic acid (26.8 g.), N,N,N',N'-tetramethyl-m-phenylenediamine (16.4 g.) and acetic anhydride (80 g.) was heated (to 95° C.) during one hour, cooled and poured into dilute hydrochloric acid. The resulting mixture was basified. Recrystallization of the resulting solid from a mixture of toluene and hexane afforded 3-(2,4-bis(dimethylamino)phenyl)-3-(4-(dimethylamino)phenyl)phthalide (I: X=Y4 =(CH3)2N, Y2 =Z4 =Z5 =Z6 =Z7 =H) (m.p. 190°-194° C.).

후처리

  1. temperaturecooled
  2. customRecrystallization of the resulting solid
  3. additionfrom a mixture of toluene and hexane

출처 및 근거

ORD 기록
ord-f064d3df4da644fe9118044c211883d6
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220357

연결된 노트

불러오는 중…