Pyridine → HCID 51109753, 화합물

HRID 633698

반응식

HRID 633698 반응식
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]

참가 물질

7

반응물 3

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

생성물 1

HCID 51109753HCID 51109753, 화합물수율 98.9%

시약·촉매·용매 3

HCID 1140Toluene용매HCID 6344Dichloromethane용매2회HCID 516892Sodium Bicarbonate용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-31d42ef2e01f42079414ff88fdf1d682
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321790B2

연결된 노트

불러오는 중…