Potassium Phosphate, Tribasic → HCID 59477832, 화합물

HRID 570846

반응식

HRID 570846 반응식
[C:1]1([C:7]2[C:8]([C:12]#[N:13])=[CH:9][NH:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:14]([O:16][C:17](=[O:25])[C:18]1[CH:23]=[CH:22][N:21]=[C:20](Br)[CH:19]=1)[CH3:15].P([O-])([O-])([O-])=O.[K+].[K+].[K+].CN[C@@H]1CCCC[C@H]1NC>C1(C)C=CC=CC=1.[Cu](I)I>[CH2:14]([O:16][C:17](=[O:25])[C:18]1[CH:19]=[CH:20][N:21]=[C:22]([N:10]2[CH:11]=[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:8]([C:12]#[N:13])=[CH:9]2)[CH:23]=1)[CH3:15]

참가 물질

7

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 2733821trans-N,N'-dimethyl-1,2-cyclohexanediamineHCID 37214604-Phenyl-1H-pyrrole-3-carbonitrileHCID 3847769Ethyl 2-bromoisonicotinate

생성물 1

HCID 59477832HCID 59477832, 화합물수율 35%

시약·촉매·용매 2

HCID 83717Copper iodide촉매HCID 1140Toluene용매

반응 조건

온도
110 °C

실험 절차

To a solution of 4-phenyl-1H-pyrrole-3-carbonitrile (0.1 g) in toluene (0.70 mL) were added 2-bromo-isonicotinic acid ethyl ester (0.19 g), potassium phosphate (0.31 g), (1R,2R)-(−)-N,N′-dimethylcyclohexane-1,2-diamine (0.02 g) and copper iodide (0.007 g) at room temperature, and this mixture was stirred at 110° C. for 24 hours. The insoluble material was removed by filtration through Celite, and this filtrate was concentrated. This obtained residue was purified by column chromatography on silica gel (eluent: ethyl acetate/n-hexane=10/90-66/34) to give the title compound (0.066 g).

후처리

  1. customThe insoluble material was removed by filtration through Celite
  2. concentrationthis filtrate was concentrated
  3. customThis obtained residue was purified by column chromatography on silica gel (eluent: ethyl acetate/n-hexane=10/90-66/34)

출처 및 근거

ORD 기록
ord-fea73fa641114481b0084c1ccb5dd478
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09023882B2

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