Sodium Carbonate → HCID 9927715, 화합물

HRID 2379729노트

반응식

HRID 2379729 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 9927715HCID 9927715, 화합물

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cdc3b32fa47a43b782dae096eb6e91e5
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05364867

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