Potassium Carbonate → HCID 78992995, 화합물

HRID 1504595노트

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HRID 1504595 반응식
Cl[C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][N:3]=1.[NH:11]1[CH2:14][CH:13]([OH:15])[CH2:12]1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[OH:15][CH:13]1[CH2:14][N:11]([C:2]2[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][N:3]=2)[CH2:12]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 804566-ChloronicotinamideHCID 15142903-Hydroxyazetidine

생성물 1

HCID 78992995HCID 78992995, 화합물수율 25.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
125 °C

실험 절차

To a solution of 6-chloronicotinamide (0.16 g, 1 mmol) and azetidin-3-ol (73 mg, 1 mmol) in DMF (5 ml) under nitrogen was added K2CO3 (0.41 g, 3 mmol). The resulting solution was stirred under nitrogen at 125° C. for 24 h. After all the starting materials were consumed, the reaction mixture was allowed to cool to ambient temperature. The reaction mixture was then filtered and the filter cake was washed with ethyl acetate. The combined filtrates were concentrated to afford the title compound (50 mg, 25%) as a yellow solid. [LCMS RtA=0.81 min, [M+H]+=194.1].

후처리

  1. customAfter all the starting materials were consumed
  2. temperatureto cool to ambient temperature
  3. filtrationThe reaction mixture was then filtered
  4. washthe filter cake was washed with ethyl acetate
  5. concentrationThe combined filtrates were concentrated

출처 및 근거

ORD 기록
ord-df7dc700cbb94f0fae475e32b9162eb5
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09216182B2

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