Water → HCID 67084484, 화합물

HRID 595199노트

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HRID 595199 반응식
C([O-])([O-])=O.[Cs+].[Cs+].[Br:7][C:8]1[CH:9]=[N:10][NH:11][CH:12]=1.Cl[CH2:14][CH:15]1[CH2:19][O:18][C:17]([CH3:21])([CH3:20])[O:16]1.O>CN(C=O)C.CCOC(C)=O>[Br:7][C:8]1[CH:9]=[N:10][N:11]([CH2:14][CH:15]2[CH2:19][O:18][C:17]([CH3:21])([CH3:20])[O:16]2)[CH:12]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 163754-BromopyrazoleHCID 203744-(Chloromethyl)-2,2-dimethyl-1,3-dioxolane

생성물 1

HCID 67084484HCID 67084484, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
65 °C

실험 절차

Cs2CO3 (5.3 g, 16.3 mmol) was added to a solution of 4-bromo-1H-pyrazole (2 g, 13.6 mmol) in DMF (10 mL), followed by 4-(chloromethyl)-2,2-dimethyl-1,3-dioxolane (2.46 g, 16.3 mmol) and the resulting mixture heated to an internal temperature of 65° C. After stirring for 14 h, water and EtOAc was added and the layers separated. The organic layer was washed a second time with water, dried with over anhydorus magnesium sulfate, filtered and concentrated under reduced pressure. The resulting crude residue was absorbed on silica gel and purified by column chromatography on silica (0 to 100% EtOAc/Hex) to afford 4-bromo-1-((2,2-dimethyl-1,3-dioxolan-4-yl)methyl)-1H-pyrazole as a light yellow oil, MS ESI calcd. for C9H14BrN2O2 [M+H]+ 261. found 261.

후처리

  1. customthe layers separated
  2. washThe organic layer was washed a second time with water
  3. dry with materialdried with over anhydorus magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting crude residue was absorbed on silica gel
  7. custompurified by column chromatography on silica (0 to 100% EtOAc/Hex)

출처 및 근거

ORD 기록
ord-ab9489696be3469d873d56cce9da4507
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242984B2

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