Hydrochloric Acid → HCID 23113375, 화합물

HRID 2102259노트

반응식

HRID 2102259 반응식
[Br:1][C:2]1[N:6]([CH:7]([CH3:9])[CH3:8])[N:5]=[C:4]([OH:10])[C:3]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12].C(=O)([O-])[O-].[K+].[K+].[CH2:22](Br)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.Cl>CN(C)C=O>[CH2:22]([O:10][C:4]1[C:3]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[C:2]([Br:1])[N:6]([CH:7]([CH3:9])[CH3:8])[N:5]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 178470082HCID 178470082, 화합물

생성물 1

HCID 23113375HCID 23113375, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Ethyl 5-bromo-3-hydroxy-1-isopropylpyrazole-4-carboxylate (5.8 g) and potassium carbonate (3.5 g) were suspended in N,N-dimethylformamide (50 mL) and to the stirred suspension was added benzyl bromide (2.76 mL) under ice cooling. The mixture was stirred at room temperature for 6 hours. The reaction mixture was poured into 1 mol/L hydrochloric acid (100 mL) and the mixture was extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the obtained residue was purified by column chromatography on silica gel (eluent: ethyl acetate/hexane=1/5) to give 7.7 g of the title compound.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe obtained residue was purified by column chromatography on silica gel (eluent: ethyl acetate/hexane=1/5)

출처 및 근거

ORD 기록
ord-734388e1ec3449abbc6311f085b6585c
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576064B2

반응 노트

불러오는 중…