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Methanol → methyl 2-[(4,6-dimethoxytriazin-2-y1)oxy]-6-[1-(N-methoxyimino)ethyl]benzoate

HRID 4908
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HRID 4908 반응식
[C:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][N:15]2[N:20]=[C:19]([O:21][CH3:22])[CH:18]=[C:17]([O:23][CH3:24])[NH:16]2)[C:5]=1[C:6]([O:8][CH3:9])=[O:7])(=O)[CH3:2].Cl.[CH3:26][O:27][NH2:28].C([O-])(=O)C.[K+].CO>O>[CH3:22][O:21][C:19]1[CH:18]=[C:17]([O:23][CH3:24])[NH:16][N:15]([O:14][C:10]2[CH:11]=[CH:12][CH:13]=[C:4]([C:1](=[N:28][O:27][CH3:26])[CH3:2])[C:5]=2[C:6]([O:8][CH3:9])=[O:7])[N:20]=1
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참가 물질

6

반응물 4

HCID 887MethanolHCID 517044Potassium AcetateHCID 521874O-Methylhydroxylamine hydrochlorideHCID 19089388Methyl 2-acetyl-6-[(4,6-dimethoxytriazin-2-yl)oxy]benzoate

생성물 1

HCID 86747186methyl 2-[(4,6-dimethoxytriazin-2-y1)oxy]-6-[1-(N-methoxyimino)ethyl]benzoate수율 48%

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

0.9 of methyl 2-acetyl-6-[(4,6-dimethoxytriazin-2-yl)oxy]benzoate, 0.68 g of methoxyamine hydrochloride and 0.80 g of potassium acetate were added to 30 ml of methanol, and the resultant mixture was stirred for one day and one night at room temperature. The resultant reaction liquor was poured into water, and was extracted with ethyl acetate. After washing the extracted product with water, the washed product was dried and concentrated to obtain an oily product. This was then purified by column chromatography to obtain 0.47 g of the aimed compound (melting point=131° to 135° C.) at a yield of 48%.

후처리

  1. customThe resultant reaction liquor
  2. extractionwas extracted with ethyl acetate
  3. washAfter washing the extracted product with water
  4. customthe washed product was dried
  5. concentrationconcentrated
  6. customto obtain an oily product
  7. customThis was then purified by column chromatography

출처 및 근거

ORD 기록
ord-9caf7f2af9b04e69903afed00c9e43d0
출처 데이터셋
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05242895

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