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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Methylamine → HCID 10246831、化合物

HRID 2396057
ノート
印刷プレビュー

反応式

HRID 2396057 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 10246831HCID 10246831、化合物

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ff9cb10e95894585975d1a684f9fb1ab
出典データセット
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05491144

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート