Potassium Carbonate → HCID 178446281、化合物

HRID 600587ノート

反応式

HRID 600587 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 178446281HCID 178446281、化合物収率 10%

試薬・触媒・溶媒 2

HCID 2631-Butanol溶媒HCID 962Water溶媒

反応条件

温度
165 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-4681e74ea04f4f0db06bdbd5b355703b
出典データセット
uspto-grants-2011_03
特許番号
US07902205B2

反応ノート

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