Sodium Carbonate → HCID 9927715、化合物

HRID 2379729ノート

反応式

HRID 2379729 の反応式
[C:1]1([C:7]2([C:13](=[O:16])[CH2:14][CH3:15])[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[CH2:18][CH2:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)CCC>[C:1]1([C:7]2([C:13](=[O:16])[CH2:14][CH3:15])[CH2:8][CH2:9][N:10]([CH2:18][CH2:19][CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:11][CH2:12]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 12503(3-Bromopropyl)benzeneHCID 1979401-(4-Phenylpiperidin-4-yl)propan-1-one

生成物 1

HCID 9927715HCID 9927715、化合物

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

6 g 4-phenyl-4-propionylpiperidine and 3.6 ml 1-bromo-3-phenylpropane was refluxed in 500 ml n-butanol with 10 g sodium carbonate for 16 hours. The reaction mixture was filtered through a silica plug and concentrated in vacuo. The residue was taken up in ethyl acetate and washed with water, then saturated brine and dried over potassium carbonate. The solution was concentrated in vacuo, 8 g of the residue was taken up in 150 ml acetonitrile and heated with 2.5 g fumaric acid. The resulting precipitate was collected by filtration, giving 3 g 4-phenyl-1-(3-phenylpropyl)-4-propionylpiperidine as the fumarate salt, melting point 136°-138° C.

後処理

  1. filtrationThe reaction mixture was filtered through a silica plug
  2. concentrationconcentrated in vacuo
  3. washwashed with water
  4. dry with materialsaturated brine and dried over potassium carbonate
  5. concentrationThe solution was concentrated in vacuo, 8 g of the residue
  6. temperatureheated with 2.5 g fumaric acid
  7. filtrationThe resulting precipitate was collected by filtration

出典と根拠

ORDレコード
ord-cdc3b32fa47a43b782dae096eb6e91e5
出典データセット
uspto-grants-1994_11
特許番号
US05364867

反応ノート

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