Potassium Carbonate → HCID 178484441, 화합물

HRID 2172677노트

반응식

HRID 2172677 반응식
[C:1]([C:3]1[CH:13]=[CH:12][C:6]([C:7]([N:9]([CH3:11])[CH3:10])=[O:8])=[CH:5][CH:4]=1)#[N:2].C(=O)([O-])[O-].[K+].[K+].Cl.[NH2:21][OH:22]>CCO.CCOC(C)=O>[OH:22][NH:21][C:1]([C:3]1[CH:13]=[CH:12][C:6]([C:7]([N:9]([CH3:11])[CH3:10])=[O:8])=[CH:5][CH:4]=1)=[NH:2]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 162277964-Cyano-N,N-dimethylbenzamide

생성물 1

HCID 178484441HCID 178484441, 화합물수율 79%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

4-cyano-N,N-dimethylbenzamide (200 mg, 1.148 mmol), potassium carbonate (952 mg, 6.89 mmol) and hydroxylamine hydrochloride (479 mg, 6.89 mmol) were dissolved in EtOH (11.4 mL). The reaction mixture was stirred at 80° C. for 25 h. The mixture was diluted with EtOAc (50 mL), washed with water (10 mL), water phase extracted with EtOAc (20 mL). Combined organic phases were washed with brine (10 mL) and dried over sodium sulfate. The solvent was removed to give 188 mg of white crystalline needles. The crude material was used without further purification.

후처리

  1. washwashed with water (10 mL), water phase
  2. extractionextracted with EtOAc (20 mL)
  3. washCombined organic phases were washed with brine (10 mL)
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed

출처 및 근거

ORD 기록
ord-5d180c150ed044609ff387b770a67238
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056843B2

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