Ammonia → HCID 23499219、化合物

HRID 361398

反応式

HRID 361398 の反応式
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4](=O)[CH2:3]1.C[N:10]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=C([N+]([O-])=O)C1=O.N>>[CH3:1][CH:2]1[CH2:3][C:4]2[N:10]=[CH:15][C:14]([N+:16]([O-:18])=[O:17])=[CH:13][C:5]=2[CH2:6][CH2:7]1

参加物

4

反応物 3

HCID 222AmmoniaHCID 115673-MethylcyclohexanoneHCID 36212361-Methyl-3,5-dinitro-1H-pyridin-2-one

生成物 1

HCID 23499219HCID 23499219、化合物収率 63%

実験手順

3-Methylcyclohexanone (0.56 g, 4.99 mmol) was mixed with 1-methyl-3,5-dinitro-2-pyridone (1.00 g, 5.02 mmol) in 1M methanolic ammonia (50 mL, 50 mmol) and heated at reflux overnight. The solvent was evaporated off and the residue was suspended in CHCl3 and flash chromatographed over silica gel (43 g) eluting with EtOAc/hexane (1:10) to afford a white solid (515 mg, 63% yield): mp 55°-56° C.

後処理

  1. temperatureheated
  2. temperatureat reflux overnight
  3. customThe solvent was evaporated off
  4. customflash chromatographed over silica gel (43 g)
  5. washeluting with EtOAc/hexane (1:10)

出典と根拠

ORDレコード
ord-13de913f451144cd924cfe70ddbe691b
出典データセット
uspto-grants-1999_02
特許番号
US05866579

関連ノート

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