Hydroxyamine hydrochloride → HCID 136337818, 화합물

HRID 552665노트

반응식

HRID 552665 반응식
[CH:1]([C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][CH:10]=[N:11][O:12][CH3:13])=[O:8])=[C:5]([CH3:16])[CH:4]=1)=O.Cl.[OH:18][NH2:19]>CO.O>[OH:18][N:19]=[CH:1][C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][CH:10]=[N:11][O:12][CH3:13])=[O:8])=[C:5]([CH3:16])[CH:4]=1

참가 물질

5

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 1363378174-formyl-N-(methoxyiminomethyl)-2-methyl benzoic acid amide

생성물 1

HCID 136337818HCID 136337818, 화합물수율 102.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

In a solution of 64 mg of 4-formyl-N-(methoxyiminomethyl)-2-methyl benzoic acid amide in 4 mL of methanol and 1 mL of water, 30 mg of hydroxyamine hydrochloride was added at room temperature with stirring, and continued to stir at the same temperature for 1.5 hour. After the completion of the reaction, 10 mL of water was added in the reaction mixture, and extracted with ethyl acetate (10 mL×2). The combined organic phases were dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified with silica gel column chromatography that were eluated with ethyl acetate-hexane (1:1) to obtain 70 mg of the aimed product as white crystal.

후처리

  1. stirringto stir at the same temperature for 1.5 hour
  2. additionwas added in the reaction mixture
  3. extractionextracted with ethyl acetate (10 mL×2)
  4. dry with materialdried over saturated sodium chloride aqueous solution
  5. distillationanhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure
  6. customThe residue was purified with silica gel column chromatography that

출처 및 근거

ORD 기록
ord-4edbc034256c4d76a599adab781fe1c5
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07951828B1

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