Potassium Carbonate → HCID 68690147、化合物

HRID 2245336ノート

反応式

HRID 2245336 の反応式
[I-].C([N+]1(C)[CH2:14][CH2:13][C:12](=[O:15])[CH:11]([CH2:16][CH2:17][CH2:18][CH3:19])[CH2:10]1)C1C=CC=CC=1.[CH3:21][O:22][C:23]1[CH:24]=[C:25]([CH:27]=[C:28]([O:32][CH3:33])[C:29]=1[O:30][CH3:31])[NH2:26].C(=O)([O-])[O-].[K+].[K+]>O.C(O)C>[CH2:16]([CH:11]1[C:12](=[O:15])[CH2:13][CH2:14][N:26]([C:25]2[CH:27]=[C:28]([O:32][CH3:33])[C:29]([O:30][CH3:31])=[C:23]([O:22][CH3:21])[CH:24]=2)[CH2:10]1)[CH2:17][CH2:18][CH3:19]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 322853,4,5-TrimethoxyanilineHCID 86605588HCID 86605588、化合物

生成物 1

HCID 68690147HCID 68690147、化合物収率 204.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

A slurry of 1-benzyl-3-butyl-1-methyl-4-oxo-piperidinium iodide (306 mg) in water (2 ml) was added in one portion to a refluxing solution of 3,4,5-trimethoxy aniline (929 mg) and anhydrous potassium carbonate (33 mg) in ethanol (4 ml). The dark solution was heated to reflux for three hours. Water was added and the reaction was extracted twice with DCM. The combined organic layers were dried over sodium sulfate, filtered and the solvent was evaporated to leave a dark oil, which was purified by flash chromatography (ethyl acetate/hexanes 1:1) to give the product as a colorless oil (520 mg). MS (ESI): 322.4 (MH+).

後処理

  1. temperatureThe dark solution was heated
  2. temperatureto reflux for three hours
  3. extractionthe reaction was extracted twice with DCM
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. customthe solvent was evaporated
  7. customto leave a dark oil, which
  8. customwas purified by flash chromatography (ethyl acetate/hexanes 1:1)

出典と根拠

ORDレコード
ord-4d9791eba0f34d24ae92b2388f259968
出典データセット
uspto-grants-2010_03
特許番号
US07683079B2

反応ノート

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