반응 #55287

ord-61d7ac485ebb41cead0d0ac85fed42d1

반응 방정식

O=C1OC(=O)c2ccccc21
phthalic anhydride
CCN(CC)c1cccc(C)c1
N,N-diethyl-m-toluidine
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
Clc1ccccc1
chlorobenzene
Clc1ccccc1
chlorobenzene
CCN(CC)c1ccc(C(=O)c2ccccc2C(=O)O)c(C)c1
2-(2-methyl-4-(diethylamino)benzoyl)benzoic acid

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04220357uspto-grants-1980_09