吡啶 → N-Methoxy-N,4-dimethyloxazole-5-carboxamide

HRID 2794

反应方程式

HRID 2794 反应方程式
[CH3:1][C:2]1[N:3]=[CH:4][O:5][C:6]=1[C:7](Cl)=[O:8].Cl.[CH3:11][NH:12][O:13][CH3:14].N1C=CC=CC=1.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[CH3:14][O:13][N:12]([CH3:11])[C:7]([C:6]1[O:5][CH:4]=[N:3][C:2]=1[CH3:1])=[O:8]

参与物

6

反应物 4

HCID 1049吡啶HCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 516892碳酸氢钠HCID 27952174-甲基恶唑-5-羰酰氯

产物 1

HCID 18925369N-Methoxy-N,4-dimethyloxazole-5-carboxamide

试剂、催化剂与溶剂 1

HCID 6212三氯甲烷溶剂

实验过程

4-Methyl-5-oxazolecarbonyl chloride (15 g) and N,O-dimethylhydroxylamine hydrochloride (11 g) in dry chloroform (100 ml) were cooled to 0° C. and dry pyridine (28.5 g) was added. The mixture was allowed to warm to room temperature. After 30 minutes aqueous sodium hydrogen carbonate was added and the organic layer separated. The aqueous layer was extracted with dichloromethane. The combined organic layers were washed, dried and evaporated. The residue was purified by flash chromatography to yield the title compound as a white solid. M.p. 59°-60° C.

后处理

  1. customthe organic layer separated
  2. extractionThe aqueous layer was extracted with dichloromethane
  3. washThe combined organic layers were washed
  4. customdried
  5. customevaporated
  6. customThe residue was purified by flash chromatography

来源与证据

ORD记录
ord-b9c8478b753b4132a133ace38f7e208b
来源数据集
uspto-grants-1998_03
专利号
US05731335

关联笔记

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