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

HRID 344570노트

반응식

HRID 344570 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

반응 조건

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 desired 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. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel chromatography (developer: n-hexane:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-7865867b5b3b409680b85909638800ac
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05053070

반응 노트

불러오는 중…