Acetone → 1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one

HRID 492123

반응식

HRID 492123 반응식
[H-].[Na+].C1COCC1.[CH3:8][O:9][C:10]1[CH:15]=[C:14]([O:16][CH3:17])[N:13]=[C:12](S(C)(=O)=O)[N:11]=1.[CH3:22][C:23]([CH3:25])=[O:24]>O>[CH3:8][O:9][C:10]1[CH:15]=[C:14]([O:16][CH3:17])[N:13]=[C:12]([CH2:22][C:23](=[O:24])[CH3:25])[N:11]=1

참가 물질

6

반응물 4

HCID 180AcetoneHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 8383634,6-Dimethoxy-2-(methylsulfonyl)pyrimidine

생성물 1

HCID 112640521-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one수율 22.4%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
30 °C

실험 절차

In a reactor were placed 16.0 g (0.4 moles) of 60% sodium hydride, 400 ml of THF and 43.6 g (0.2 moles) of 4,6-dimethoxy-2-methanesulfonylpyrimidine. The reactor contents were heated to 30° C. Thereto was dropwise added 39.4 g (0.68 moles) of acetone, followed by a reaction for 2 hours. After the completion of the reaction, 350 ml of water was added and extraction with 500 ml of ethyl acetate was conducted. The ethyl acetate layer was concentrated. The concentrate was subjected to distillation under reduced pressure to obtain 8.8 g (44.9 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone. Refractive index n20D: 1.5181

후처리

  1. customIn a reactor were placed
  2. customfollowed by a reaction for 2 hours
  3. additionwas added
  4. extractionextraction with 500 ml of ethyl acetate
  5. concentrationThe ethyl acetate layer was concentrated
  6. distillationThe concentrate was subjected to distillation under reduced pressure

출처 및 근거

ORD 기록
ord-d11dc1e038e34defa51bd8a541a25166
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531654B2

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