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Hydroxyamine hydrochloride → methyl N-[4-hydroxyiminomethyl-2-methylbenzoyl]carbamate

HRID 1187999
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HRID 1187999 반응식
[CH:1]([C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][C:10](=[O:13])[O:11][CH3:12])=[O:8])=[C:5]([CH3:16])[CH:4]=1)=O.Cl.[NH2:18][OH:19]>CO.O>[OH:19][N:18]=[CH:1][C:3]1[CH:15]=[CH:14][C:6]([C:7]([NH:9][C:10](=[O:13])[O:11][CH3:12])=[O:8])=[C:5]([CH3:16])[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 86654470methyl N-[4-formyl-2-methyl benzoyl]carbamate

생성물 1

HCID 86654469methyl N-[4-hydroxyiminomethyl-2-methylbenzoyl]carbamate수율 102.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

In a solution of 41 mg of methyl N-[4-formyl-2-methyl benzoyl]carbamate in 4 mL of methanol and 1 mL of water, 15 mg of hydroxylamine 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 to obtain 45 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

출처 및 근거

ORD 기록
ord-fdbe860e59ad4bf9bee204ee1968de82
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08673951B2

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