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

HRID 915539

反応式

HRID 915539 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-6e42b245ec7a42478dab5d862e88db9b
出典データセット
uspto-grants-2007_09
特許番号
US07265227B2

関連ノート

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