Benzenecarboximidic acid, ethyl ester, hydrochloride (1:1) → HCID 21098365、化合物

HRID 713410

反応式

HRID 713410 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([NH:16][NH2:17])=[O:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.C(O[C:22](=N)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)C>CCO>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[O:15][C:22]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[N:17][N:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 2

HCID 79249Benzenecarboximidic acid, ethyl ester, hydrochloride (1:1)HCID 22713165tert-Butyl 4-(hydrazinecarbonyl)piperidine-1-carboxylate

生成物 1

HCID 21098365HCID 21098365、化合物収率 20.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution of 4-hydrazinocarbonyl-piperidine-1-carboxylic acid tert-butyl ester (1.15 g, 4.73 mmol, 1.0 eq) in EtOH (15 mL) was added benzimidic acid ethyl ester hydrochloride (921 mg, 4.96 mmol, 1.05 eq.) and the reaction mixture was refluxed for 48 h. The inorganic precipitate was filtered off, washed with ethyl acetate, and the solvent of the mother liquor was evaporated in vacuo. The residue was purified by column chromatography (ethyl acetate/heptanes) to give the title compound as a white solid (327 mg, 0.99 mmol). MS (m/z, MH+): 330.2

後処理

  1. temperaturethe reaction mixture was refluxed for 48 h
  2. filtrationThe inorganic precipitate was filtered off
  3. washwashed with ethyl acetate
  4. customthe solvent of the mother liquor was evaporated in vacuo
  5. customThe residue was purified by column chromatography (ethyl acetate/heptanes)

出典と根拠

ORDレコード
ord-fef1ec9c13244d4393c3ab5c1ec1c115
出典データセット
uspto-grants-2015_11
特許番号
US09181266B2

関連ノート

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