Phthalic Anhydride → 2-(4-(Diethylamino)-2-methylbenzoyl)benzoic acid

HRID 27009

반응식

HRID 27009 반응식
[C:1]1(=[O:11])[O:6][C:4](=[O:5])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.[CH2:12]([N:14]([CH2:22][CH3:23])[C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([CH3:21])[CH:16]=1)[CH3:13].[Cl-].[Al+3].[Cl-].[Cl-].ClC1C=CC=CC=1>O>[CH3:21][C:17]1[CH:16]=[C:15]([N:14]([CH2:12][CH3:13])[CH2:22][CH3:23])[CH:20]=[CH:19][C:18]=1[C:4]([C:3]1[CH:7]=[CH:8][CH:9]=[CH:10][C:2]=1[C:1]([OH:6])=[O:11])=[O:5]

참가 물질

6

반응물 4

HCID 6811Phthalic AnhydrideHCID 7964Chlorobenzene2회HCID 66679N,N-diethyl-m-toluidineHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 1043352-(4-(Diethylamino)-2-methylbenzoyl)benzoic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of phthalic anhydride (60 g.), N,N-diethyl-m-toluidine (162.8 g.), aluminum chloride (120 g.) and chlorobenzene (360 ml.) was heated (75°-95° C.) during one and one-half hours, then diluted with water (200 ml., then more). More chlorobenzene (200 ml.) was added and the chlorobenzene layer was separated and steam distilled. Addition of sodium hydroxide solution (10%) to a solution of the residue in dilute sulfuric acid (20%, 250 ml.) afforded 2-(2-methyl-4-(diethylamino)benzoyl)benzoic acid (IV: Y2 =CH3, Y'4 =(CH3CH2)2N, Z4 =Z"5 =Z"6 =Z7 =H).

후처리

  1. temperaturewas heated (75°-95° C.) during one and one-half hours
  2. customthe chlorobenzene layer was separated
  3. distillationsteam distilled
  4. additionAddition of sodium hydroxide solution (10%) to a solution of the residue in dilute sulfuric acid (20%, 250 ml.)

출처 및 근거

ORD 기록
ord-61d7ac485ebb41cead0d0ac85fed42d1
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220357

연결된 노트

불러오는 중…