Pyridine → HCID 51109753、化合物

HRID 633698

反応式

HRID 633698 の反応式
N1C=CC=CC=1.Cl.[CH3:8][NH:9][O:10][CH3:11].[CH3:12][C:13]1[C:17]([C:18](Cl)=[O:19])=[C:16]([CH3:21])[O:15][N:14]=1>ClCCl.C([O-])(O)=O.[Na+].C1(C)C=CC=CC=1>[CH3:11][O:10][N:9]([CH3:8])[C:18]([C:17]1[C:13]([CH3:12])=[N:14][O:15][C:16]=1[CH3:21])=[O:19]

参加物

7

反応物 3

HCID 1049PyridineHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 27362653,5-Dimethylisoxazole-4-carbonyl Chloride

生成物 1

HCID 51109753HCID 51109753、化合物収率 98.9%

試薬・触媒・溶媒 3

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒2 回HCID 516892Sodium Bicarbonate溶媒

実験手順

659 μl (8.15 mmol) of pyridine are added to a suspension of 343.07 mg (3.45 mmol) of N,O-dimethylhydroxylamine hydrochloride in 10 mL of dichloromethane. The mixture is stirred at room temperature until fully dissolved. A solution of 526.32 mg (3.13 mmol) of 3,5-dimethylisoxazole-4-carbonyl chloride in 5 mL of dichloromethane is then added. After stirring for 1 hour at room temperature, the reaction mixture is taken up in saturated aqueous NaHCO3 solution and stirred for a few minutes, and the phases are separated by settling. The organic phase is dried over magnesium sulfate and evaporated to dryness. The residue obtained is taken up in toluene and evaporated, the operation being repeated a second time. 570 mg of N-methoxy-N-methyl-3,5-dimethylisoxazole-4-carboxamide are then obtained, corresponding to the following characteristics:

後処理

  1. dissolutionuntil fully dissolved
  2. stirringAfter stirring for 1 hour at room temperature
  3. stirringstirred for a few minutes
  4. customthe phases are separated
  5. dry with materialThe organic phase is dried over magnesium sulfate
  6. customevaporated to dryness
  7. customThe residue obtained
  8. customevaporated

出典と根拠

ORDレコード
ord-31d42ef2e01f42079414ff88fdf1d682
出典データセット
uspto-grants-2016_04
特許番号
US09321790B2

関連ノート

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