Benzenecarboximidic acid, ethyl ester, hydrochloride (1:1) → HCID 21098365, 화합물

HRID 713410

반응식

HRID 713410 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 21098365HCID 21098365, 화합물수율 20.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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

후처리

  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)

출처 및 근거

ORD 기록
ord-fef1ec9c13244d4393c3ab5c1ec1c115
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181266B2

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