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

HRID 437865

反応式

HRID 437865 の反応式
[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]

参加物

6

反応物 4

HCID 6811Phthalic AnhydrideHCID 7964Chlorobenzene2 回HCID 66679N,N-diethyl-m-toluidineHCID 6451240Aluminum(III) Chloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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.)

出典と根拠

ORDレコード
ord-c838bc84aeed453ca7bf0e4e8d147cdf
出典データセット
uspto-grants-1977_06
特許番号
US04032527

関連ノート

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