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

HRID 27012

반응식

HRID 27012 반응식
[CH3:1][N:2]([CH3:23])[C:3]1[CH:19]=[C:18]([N:20]([CH3:22])[CH3:21])[CH:17]=[CH:16][C:4]=1[C:5]([C:7]1[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=1[C:9]([OH:11])=O)=[O:6].[CH3:24][N:25]([CH3:35])[C:26]1[CH:31]=[CH:30][CH:29]=[C:28]([N:32]([CH3:34])[CH3:33])[CH:27]=1.C(OC(=O)C)(=O)C.Cl>>[CH3:33][N:32]([CH3:34])[C:28]1[CH:27]=[C:26]([N:25]([CH3:35])[CH3:24])[CH:31]=[CH:30][C:29]=1[C:5]1([C:4]2[CH:16]=[CH:17][C:18]([N:20]([CH3:22])[CH3:21])=[CH:19][C:3]=2[N:2]([CH3:1])[CH3:23])[C:7]2[C:8](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:9](=[O:11])[O:6]1

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 897151,3-Benzenediamine, N1,N1,N3,N3-tetramethyl-HCID 202872122-(2,4-Bis(dimethylamino)benzoyl)benzoic acid

생성물 1

HCID 202165793,3-Bis(2,4-bis(dimethylamino)phenyl)phthalide

실험 절차

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.).

후처리

  1. temperaturewas warmed (at 25°-35° C.) during two to three hours
  2. filtrationfiltered with a filter aid
  3. extractionThe filter cake was extracted with hot toluene
  4. extractionDilution of the toluene extract with hexane

출처 및 근거

ORD 기록
ord-26a60b8ba57e4627874ea4144aa19bfb
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220357

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