Potassium Carbonate → HCID 178451398, 화합물

HRID 733422노트

반응식

HRID 733422 반응식
[C:1]([O:5][C:6]([N:8]1[CH:13]2[CH2:14][CH2:15][CH:9]1[CH2:10][CH:11]([CH:16]1[C:29]3[CH:28]=[CH:27][C:26]([C:30]#[N:31])=[CH:25][C:24]=3[O:23][C:22]3[C:17]1=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH2:12]2)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.NO.C(=O)([O-])[O-].[K+].[K+].Cl.[OH-:42].[NH4+:43]>C(O)C.O>[C:1]([O:5][C:6]([N:8]1[CH:9]2[CH2:15][CH2:14][CH:13]1[CH2:12][CH:11]([CH:16]1[C:29]3[CH:28]=[CH:27][C:26]([C:30](=[NH:43])[NH:31][OH:42])=[CH:25][C:24]=3[O:23][C:22]3[C:17]1=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH2:10]2)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

7

반응물 4

HCID 11430Potassium Carbonate2회HCID 443297Hydroxyamine hydrochlorideHCID 13908798HCID 13908798, 화합물HCID 578392203-(3-cyano-9H-xanthen-9-yl)-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester

생성물 1

HCID 178451398HCID 178451398, 화합물수율 102%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of 3-(3-cyano-9H-xanthen-9-yl)-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (635 mg; 0.877 mmol) in ethanol (10 mL) was added hydroxylamine hydrochloride (183 mg; 2.62 mmol) and potassium carbonate (242 mg; 1.75 mmol), and the mixture was heated to reflux for 16 h. More ammonium hydroxide hydrochloride (183 mg; 2.62 mmol) and potassium carbonate (242 mg; 1.75 mmol) were added, and the mixture was heated to reflux for 24 h. The mixture was allowed to cool to rt, water was added, and the solid was collected by filtration, yielding 402 mg (quant.) of 3-[3-(N-hydroxycarbamimidoyl)-9H-xanthen-9-yl]-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester, 1n. The crude material was used as such in the next reaction.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 16 h
  3. temperaturethe mixture was heated
  4. temperatureto reflux for 24 h
  5. filtrationthe solid was collected by filtration

출처 및 근거

ORD 기록
ord-46291a43213e42a3af44200c1a6b9079
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07589104B2

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