Hydrochloric Acid → Amino-5,6-dichloro-3-nitrobenzoic acid

HRID 487195

反応式

HRID 487195 の反応式
[N+:1]([C:4]1[C:5](Cl)=[C:6]([C:10]([Cl:14])=[C:11]([Cl:13])[CH:12]=1)[C:7]([OH:9])=[O:8])([O-:3])=[O:2].ClC1C=CC=CC=1C[NH2:20].Cl>C1(C)C=CC=CC=1>[NH2:20][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:12][C:11]([Cl:13])=[C:10]([Cl:14])[C:6]=1[C:7]([OH:9])=[O:8]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 666482-ChlorobenzylamineHCID 190942393-Nitro-2,5,6-trichlorobenzoic acid

生成物 1

HCID 131718350Amino-5,6-dichloro-3-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a stirred solution of 3-nitro-2,5,6-trichlorobenzoic acid (37.1 mmol, 10.0 g) in 150 mL of toluene, was added 2-chlorobenzylamine (81.6 mmol, 11.56 g). The reaction mixture was refluxed overnight, poured into dilute hydrochloric acid and vigorously stirred. The resulting solid was filtered. The product was dissolved in toluene and then precipitated with diethyl ether. Recrystallization of the product from methanol gave 3.4 g of 2-[2-chlorophenyl)methyl]amino-5,6-dichloro-3-nitrobenzoic acid; mp 168.5°-171° C.

後処理

  1. temperatureThe reaction mixture was refluxed overnight
  2. filtrationThe resulting solid was filtered
  3. dissolutionThe product was dissolved in toluene
  4. customprecipitated with diethyl ether
  5. customRecrystallization of the product from methanol

出典と根拠

ORDレコード
ord-2acbb49479fc4ff59a140401e97e8c33
出典データセット
uspto-grants-1994_03
特許番号
US05294631

関連ノート

読み込み中…