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

HRID 2794

反応式

HRID 2794 の反応式
[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]

参加物

6

反応物 4

HCID 1049PyridineHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 516892Sodium BicarbonateHCID 27952174-Methyloxazole-5-carbonyl chloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b9c8478b753b4132a133ace38f7e208b
出典データセット
uspto-grants-1998_03
特許番号
US05731335

関連ノート

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