4-Ethoxyaniline → HCID 13588352, 화합물

HRID 280266노트

반응식

HRID 280266 반응식
[CH2:1]([O:3][C:4]1[CH:10]=[CH:9][C:7]([NH2:8])=[CH:6][CH:5]=1)[CH3:2].[Cl:11][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>[Cl:11][C:12]1[C:20]([N+:21]([O-:23])=[O:22])=[CH:19][C:18]([N+:24]([O-:26])=[O:25])=[C:17]([NH:8][C:7]2[CH:9]=[CH:10][C:4]([O:3][CH2:1][CH3:2])=[CH:5][CH:6]=2)[C:13]=1[C:14]([OH:16])=[O:15]

참가 물질

5

반응물 3

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

생성물 1

HCID 13588352HCID 13588352, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1473791d83854b458cc132a6de04af60
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04588730

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