Hydrogen Peroxide → 6-氯-5-甲基吡啶-3-羧酸

HRID 1908773笔记

反应方程式

HRID 1908773 反应方程式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH:8]=[O:9])=[CH:4][C:3]=1[CH3:10].[OH:11]O>C(O)=O.O>[Cl:1][C:2]1[C:3]([CH3:10])=[CH:4][C:5]([C:8]([OH:11])=[O:9])=[CH:6][N:7]=1

参与物

5

反应物 2

HCID 784Hydrogen PeroxideHCID 197106816-氯-5-甲基吡啶-3-羧醛

产物 1

HCID 123877296-氯-5-甲基吡啶-3-羧酸

试剂、催化剂与溶剂 2

HCID 284甲酸溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次

反应条件

温度
0 °C

实验过程

A solution of 6-chloro-3-formyl-5-methyl-pyridine (10 g, 64 mmol) in formic acid (200 mL) is cooled at 0° C. and an aq. 50% weight solution of H2O2 in water (9.6 mL, 360 mmol) is added at this temperature. The mixture is stirred at 0° C. for 15 h, carefully diluted with water (200 mL) and extracted with DCM (8×100 mL). The combined org. extracts are washed with 1M aq. HCl (100 mL) (check for remaining peroxide), dried (MgSO4), filtered and evaporated. The residue is dried to give the title compound (9.56 g); LC-MS: tR=0.72 min, [M+1]+=172.0.

后处理

  1. extractionextracted with DCM (8×100 mL)
  2. washextracts are washed with 1M aq. HCl (100 mL) (check for remaining peroxide)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue is dried

来源与证据

ORD记录
ord-7686e5af131c4baf98a80d74894b3898
来源数据集
uspto-grants-2013_12
专利号
US08598208B2

反应笔记

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