碘化钠 → Methyl 4-(3,4-dichlorophenoxy)-1-piperidinebutanoate

HRID 915539笔记

反应方程式

HRID 915539 反应方程式
[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

参与物

6

反应物 4

HCID 5238碘化钠HCID 11430碳酸钾HCID 1076044-溴丁酸甲酯HCID 37320424(3,4-二氯苯氧基)哌啶

产物 1

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

试剂、催化剂与溶剂 1

HCID 180丙酮溶剂

实验过程

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).

后处理

  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)

来源与证据

ORD记录
ord-6e42b245ec7a42478dab5d862e88db9b
来源数据集
uspto-grants-2007_09
专利号
US07265227B2

反应笔记

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