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Water → methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-[1-(N-methoxyimino)ethyl]benzoate

HRID 4903
ノート
印刷プレビュー

反応式

HRID 4903 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([S:11][C:12]2[CH:21]=[CH:20][CH:19]=[C:18]([C:22](=O)[CH3:23])[C:13]=2[C:14]([O:16][CH3:17])=[O:15])[N:4]=1.Cl.[CH3:26][O:27][NH2:28].C(=O)([O-])[O-].[K+].[K+].O>CO>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([S:11][C:12]2[CH:21]=[CH:20][CH:19]=[C:18]([C:22](=[N:28][O:27][CH3:26])[CH3:23])[C:13]=2[C:14]([O:16][CH3:17])=[O:15])[N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 521874O-Methylhydroxylamine hydrochlorideHCID 19089402Methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-acetylbenzoate

生成物 1

HCID 86747183methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-[1-(N-methoxyimino)ethyl]benzoate収率 60%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

1.0 g of methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-acetylbenzoate and 0.5 g of methoxyamine hydrochloride were dissolved in 6 ml of methanol, and the resultant solution was refluxed for 15 minutes. After cooling the mixed liquor to room temperature, 0.8 g of potassium carbonate was added to this liquor and the resultant liquor was heat-refluxed for 3 hours. The reaction liquor was poured into a large amount of water, and an oily product thus precipitated was extracted with ethyl acetate. The ethyl acetate layer was washed with water, and was dried to distill off ethyl acetate under reduced pressure. The residue thus obtained was purified by chromatography to obtain 0.65 g of the aimed compound (refractive index=1.5709) at a yield of 59%.

後処理

  1. temperaturethe resultant liquor was heat-refluxed for 3 hours
  2. customan oily product thus precipitated
  3. extractionwas extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with water
  5. customwas dried
  6. distillationto distill off ethyl acetate under reduced pressure
  7. customThe residue thus obtained
  8. customwas purified by chromatography

出典と根拠

ORDレコード
ord-a7a4e504e0e84b019b4a1e1fa710be55
出典データセット
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05242895

反応ノート

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