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Methylamine → HCID 10246831, 화합물

HRID 2396057
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HRID 2396057 반응식
CO[C:3](=[O:28])[C:4]1[C:5](=[CH:10][C:11]([NH:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[C:12]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:13]=1)[C:6](OC)=[O:7].[CH3:29][NH2:30]>C(O)CO>[NH:21]([C:11]1[CH:10]=[C:5]2[C:6](=[O:7])[N:30]([CH3:29])[C:3](=[O:28])[C:4]2=[CH:13][C:12]=1[NH:14][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 10407176dimethyl 4,5-dianilinobenzene-1,2-dicarboxylate

생성물 1

HCID 10246831HCID 10246831, 화합물

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

실험 절차

Analogously to Example 1, 376 mg (1 mmol) of 4,5-bis(anilino)phthalic acid dimethyl ester in 33 ml of ethylene glycol are heated at 120° and, with stirring, methylamine is passed through the mixture for 18 hours. Thereaction mixture is cooled and extracted with ethyl acetate. The ethyl acetate phases are washed in succession three times with water and once with saturated sodium chloride solution, dried with sodium sulfate and concentrated by evaporation. The evaporation residue is chromatographed onsilica gel with hexane/ethyl acetate 1:1 and the product fractions are combined and concentrated by evaporation, yielding the title compound in the form of slightly yellow crystals, FAB-MS: 344 [M+ +H], m.p. 195°-196° C.

후처리

  1. temperatureThereaction mixture is cooled
  2. extractionextracted with ethyl acetate
  3. washThe ethyl acetate phases are washed in succession three times with water and once with saturated sodium chloride solution
  4. dry with materialdried with sodium sulfate
  5. concentrationconcentrated by evaporation
  6. customThe evaporation residue is chromatographed onsilica gel with hexane/ethyl acetate 1:1
  7. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-ff9cb10e95894585975d1a684f9fb1ab
출처 데이터셋
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05491144

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