Sodium Iodide → Methyl 4-(3,4-dichlorophenoxy)-1-piperidinebutanoate

HRID 915539

반응식

HRID 915539 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[O:5][CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].Br[CH2:25][CH2:26][CH2:27][C:28]([O:30][CH3:31])=[O:29]>CC(C)=O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[O:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:25][CH2:26][CH2:27][C:28]([O:30][CH3:31])=[O:29])[CH2:8][CH2:7]1

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 107604Methyl 4-bromobutyrateHCID 37320424-(3,4-Dichlorophenoxy)piperidine

생성물 1

HCID 69417722Methyl 4-(3,4-dichlorophenoxy)-1-piperidinebutanoate

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

4-(3,4-Dichlorophenoxy)piperidine (4.15 g) was dissolved in acetone (80 ml). Potassium carbonate (2.42 g), sodium iodide (0.49 g) and then methyl 4-bromobutyrate (1.95 ml) were added and the mixture was stirred for 42 h. The solvent, was evaporated and the residue was partitioned between water and ethyl acetate. The aqueous phase was extracted with ethyl acetate. The organic phases were dried (MgSO4), filtered and evaporated and the residue was chromatographed eluting with ethyl acetate: triethylamine (99:1) to give the subtitle compound (4.52 g).

후처리

  1. customThe solvent, was evaporated
  2. customthe residue was partitioned between water and ethyl acetate
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. dry with materialThe organic phases were dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customthe residue was chromatographed
  8. washeluting with ethyl acetate: triethylamine (99:1)

출처 및 근거

ORD 기록
ord-6e42b245ec7a42478dab5d862e88db9b
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265227B2

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