Potassium Carbonate → HCID 178446281, 화합물

HRID 2374316

반응식

HRID 2374316 반응식
[CH2:1]([NH:6][C:7]1[N:8]=[CH:9][NH:10][C:11]=1[C:12]#[N:13])[CH2:2][CH2:3][CH2:4][CH3:5].[C:14]([NH:17][NH2:18])(=O)[CH3:15].C(=O)([O-])[O-].[K+].[K+]>C(O)CCC.O>[CH3:15][C:14]1[N:13]=[C:12]([C:11]2[NH:10][CH:9]=[N:8][C:7]=2[NH:6][CH2:1][CH2:2][CH2:3][CH2:4][CH3:5])[NH:18][N:17]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 14039AcetohydrazideHCID 451205654-(pentylamino)-1H-imidazole-5-carbonitrile

생성물 1

HCID 178446281HCID 178446281, 화합물수율 10%

시약·촉매·용매 2

HCID 2631-Butanol용매HCID 962Water용매

반응 조건

온도
165 °C

실험 절차

To the mixture of 4-(pentylamino)-1H-imidazole-5-carbonitrile (0.40 g, 2 mmol), acetic acid, hydrazide (0.33 g, 4.5 mmol) in 1-butanol (10 mL) was added potassium carbonate (0.10 g, 0.72 mmol). The mixture was sealed and stirred at 165° C. for 14 hours. The reaction mixture was diluted with water and extracted with ethyl acetate three times. The combined organic layers were dried with sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by preparative LCMS (method A) to yield the desired product (45 mg, 10% yield). LCMS calculated for C11H19N6(M+H): 235.2; found: 235.1.

후처리

  1. customThe mixture was sealed
  2. extractionextracted with ethyl acetate three times
  3. dry with materialThe combined organic layers were dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by preparative LCMS (method A)

출처 및 근거

ORD 기록
ord-0a4a862f0dfc4446b09265adeb3da561
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07462624B2

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