丙酮 → 维拉帕米杂质20

HRID 405015笔记

反应方程式

HRID 405015 反应方程式
[C:1]([OH:6])(=O)[C:2](O)=O.[C:7]([C:9]1([C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[C:21]([O:27][CH3:28])[CH:20]=2)OC(CCC(C)C)CO1)#[N:8].[C:29](=O)([O-])[O-].[K+].[K+].[CH3:35][C:36]([CH3:38])=O>O>[CH3:28][O:27][C:21]1[CH:20]=[C:19]([C:9]([CH:36]([CH3:38])[CH3:35])([CH2:29][CH2:2][CH:1]=[O:6])[C:7]#[N:8])[CH:24]=[CH:23][C:22]=1[O:25][CH3:26]

参与物

6

反应物 4

HCID 180丙酮HCID 971草酸HCID 11430碳酸钾HCID 671041742-Cyano-2-(3,4-dimethoxyphenyl)-2-isopropylethyl-1,3-dioxolane

产物 1

HCID 3015370维拉帕米杂质20

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
80 °C

实验过程

Oxalic acid dehydrate (504.6 mg, 3.96 mmol) was added to a solution of the acetal (19) (372 mg, 1.16 mmol) in acetone (10 mL) and water (10 mL). The resulting mixture was stirred at 80° C. for four hours. The reaction mixture was cooled to room temperature. Potassium carbonate (1.3 g) was added to quench the reaction. The mixture was extracted with ethyl ether (3×20 mL). The organic solution was washed with brine, dried over sodium sulfate, concentrated to afford the crude product (17) (293 mg), which was used in the next step without further purification. The product was confirmed by 1H-NMR spectra.

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customto quench
  3. customthe reaction
  4. extractionThe mixture was extracted with ethyl ether (3×20 mL)
  5. washThe organic solution was washed with brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated

来源与证据

ORD记录
ord-8e15abe2e51e4aeaa373318080326d13
来源数据集
uspto-grants-2014_06
专利号
US08748648B2

反应笔记

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