Pyridine → HCID 53869643, 화합물

HRID 342181노트

반응식

HRID 342181 반응식
Cl.[CH3:2][O:3][NH2:4].N1C=CC=CC=1.[CH3:11][NH:12][C:13](=[O:30])[C:14](=O)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH2:21][O:22][CH:23]1[CH2:28][CH2:27][CH2:26][CH2:25][O:24]1>CO.[Cl-].[Na+].O>[CH3:2][O:3][N:4]=[C:14]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH2:21][O:22][CH:23]1[CH2:28][CH2:27][CH2:26][CH2:25][O:24]1)[C:13]([NH:12][CH3:11])=[O:30]

참가 물질

6

반응물 3

HCID 1049PyridineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 18357814HCID 18357814, 화합물

생성물 1

HCID 53869643HCID 53869643, 화합물수율 60.4%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 57417360Sodium chloride; water용매

실험 절차

Methoxyamine hydrochloride (0.33 g, 0.004 mol) was dissolved in methanol (4 ml), and pyridine (0.47 g, 0.006 mol) was added to the solution. To the mixture was added a mixed solution of N-methyl-2-oxo-2-[2-(2-tetrahydropyranyloxymethyl)phenyl]acetamide (0.55 g, 0.002 mol) and methanol (2 ml). The mixture was stirred under reflux for 2 hours. After completion of the reaction, half-saturated brine (100 ml) was added, and the mixture was extracted with dichloromethane (80 ml) twice. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to obtain an E/Z mixture of 2-methoxyimino-N-methyl-2-[2-(2-tetrahydropyranyloxymethyl)phenyl]acetamide (0.37 g, Yield: 60.4%) as a colorless oil.

후처리

  1. temperatureunder reflux for 2 hours
  2. additionwas added
  3. extractionthe mixture was extracted with dichloromethane (80 ml) twice
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)
  7. customto obtain

출처 및 근거

ORD 기록
ord-e6093a031e864708919aada10d14c2ab
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05856573

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