4-Ethoxyaniline → HCID 15922784、化合物

HRID 1731384ノート

反応式

HRID 1731384 の反応式
[CH2:1]([O:3][C:4]1[CH:10]=[CH:9][C:7]([NH2:8])=[CH:6][CH:5]=1)[CH3:2].Cl[C:12]1[C:20]([N+:21]([O-:23])=[O:22])=[CH:19][C:18]([N+:24]([O-:26])=[O:25])=[C:17](Cl)[C:13]=1[C:14]([OH:16])=[O:15].C(N(CC)C(C)C)(C)C>C(#N)C>[CH2:1]([O:3][C:4]1[CH:10]=[CH:9][C:7]([NH:8][C:12]2[C:13]([C:14]([OH:16])=[O:15])=[CH:17][C:18]([N+:24]([O-:26])=[O:25])=[CH:19][C:20]=2[N+:21]([O-:23])=[O:22])=[CH:6][CH:5]=1)[CH3:2]

参加物

5

反応物 3

HCID 90764-EthoxyanilineHCID 81531DiisopropylethylamineHCID 2963442,6-Dichloro-3,5-dinitrobenzoic acid

生成物 1

HCID 15922784HCID 15922784、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

A solution of 10.5 g of 4-ethoxyaniline in 250 ml acetonitrile was added over a 1.5 hour period to a solution of 20 g of 2,6-dichloro-3,5-dinitrobenzoic acid and 11 g of N,N-diisopropylethylamine in 400 ml of acetonitrile and stirred at room temperature for five hours. After the solvent was removed in vacuo, the residue was dissolved in 500 ml of chloroform and extracted with several portions of 5% ammonium hydroxide. The aqueous extracts were washed with chloroform and acidified with dilute acid. The resulting solid was collected by filtration and was washed with water to provide 2-chloro=6-[(4-ethoxyphenyl)amino]-3,5-dinitrobenzoic acid, mp 202°-206° C.

後処理

  1. customAfter the solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in 500 ml of chloroform
  3. extractionextracted with several portions of 5% ammonium hydroxide
  4. washThe aqueous extracts were washed with chloroform
  5. additionwith dilute acid
  6. filtrationThe resulting solid was collected by filtration
  7. washwas washed with water

出典と根拠

ORDレコード
ord-5e879764cf44469795bfe00e7048f7e2
出典データセット
uspto-grants-1986_11
特許番号
US04621086

反応ノート

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