Potassium Carbonate → 2-(4,6-Dimethoxy-2-pyrimidinyloxy)benzaldoxime

HRID 704294노트

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HRID 704294 반응식
Cl.[NH2:2][OH:3].C(=O)([O-])[O-].[K+].[K+].[CH3:10][O:11][C:12]1[CH:17]=[C:16]([O:18][CH3:19])[N:15]=[C:14]([O:20][C:21]2[CH:28]=[CH:27][CH:26]=[CH:25][C:22]=2[CH:23]=O)[N:13]=1>O.CO>[CH3:10][O:11][C:12]1[CH:17]=[C:16]([O:18][CH3:19])[N:15]=[C:14]([O:20][C:21]2[CH:28]=[CH:27][CH:26]=[CH:25][C:22]=2[CH:23]=[N:2][OH:3])[N:13]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 820623Benzaldehyde, 2-[(4,6-dimethoxy-2-pyrimidinyl)oxy]-

생성물 1

HCID 9021982-(4,6-Dimethoxy-2-pyrimidinyloxy)benzaldoxime수율 56%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

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온도
0 °C

실험 절차

3.5 g of hydroxylamine hydrochloride were added to 100 ml of a 1:1 mixed solution of water and methanol containing 3.5 g of potassium carbonate at 0° C. The solution was stirred at 0° C. for 10 minutes. At 0° C., 13.0 g of 2-(4,6-dimethoxy-2-pyrimidinyloxy)benzaldehyde were added to the reaction mixture. The resulting mixture was stirred at room temperature for 1 hour and then warmed at 60° C. for 1 hour. After the reaction mixture was allowed to cool down, it was poured into water, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel chromatography (developer: n-hexane:ethyl acetate=5:1) to obtain 7.7 g of 2-(4,6-dimethoxy-2-pyrimidinyloxy)benzaldoxime.

후처리

  1. stirringThe resulting mixture was stirred at room temperature for 1 hour
  2. temperaturewarmed at 60° C. for 1 hour
  3. temperatureto cool down
  4. extractionfollowed by extraction with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel chromatography (developer: n-hexane:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-6f6b57d35fa9481fb7f1c388e48b22b9
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04986846

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