Hydrochloric Acid → HCID 23113375, 화합물

HRID 1365045노트

반응식

HRID 1365045 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:7]([OH:15])=[N:8][N:9]([CH:12]([CH3:14])[CH3:13])[C:10]=1[Br:11])=[O:5])[CH3:2].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>[CH2:1]([O:3][C:4]([C:6]1[C:7]([O:15][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[N:8][N:9]([CH:12]([CH3:14])[CH3:13])[C:10]=1[Br:11])=[O:5])[CH3:2]

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

5-Bromo-3-hydroxy-1-isopropylpyrazole-4-carboxylic acid ethyl ester (5.8 g) and potassium carbonate (3.5 g) were suspended in N,N-dimethylformamide (50 mL), and benzyl bromide (2.76 mL) was added to the suspension 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 the title compound (7.7 g)

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-eb902fd995f6498abe4f7d48452f28a8
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07888487B2

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