O-Methylhydroxylamine hydrochloride → 4-bromo-N-(methoxyiminomethyl)-2-methyl benzoic acid amide

HRID 878845노트

반응식

HRID 878845 반응식
[Br:1][C:2]1[CH:14]=[CH:13][C:5]([C:6]([N:8]=[CH:9][N:10](C)C)=[O:7])=[C:4]([CH3:15])[CH:3]=1.Cl.[CH3:17][O:18]N>O1CCOCC1.O.C(OCC)(=O)C>[Br:1][C:2]1[CH:14]=[CH:13][C:5]([C:6]([NH:8][CH:9]=[N:10][O:18][CH3:17])=[O:7])=[C:4]([CH3:15])[CH:3]=1

참가 물질

6

반응물 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 666997874-Bromo-N-[(dimethylamino)methylene]-2-methylbenzamide

생성물 1

HCID 1363378164-bromo-N-(methoxyiminomethyl)-2-methyl benzoic acid amide수율 103.7%

시약·촉매·용매 3

HCID 962Water용매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

In a solution of 0.67 g of 4-bromo-N-(dimethylaminomethylidene)-2-methyl benzoic acid amide in 10 mL of 1,4-dioxane, a solution of 0.36 g of methoxyamine hydrochloride in 2 mL of water was added, and stirred at room temperature for 1 hour. After the completion of the reaction, the reaction mixture was diluted with 50 mL of ethyl acetate, washed with water, and dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 0.70 g of the aimed product as white crystal.

후처리

  1. customAfter the completion of the reaction
  2. washwashed with water
  3. dry with materialdried over saturated sodium chloride aqueous solution
  4. distillationanhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-994f2ba79c5742c2b0470eb0701ee698
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987464B2

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