Hydrochloric Acid → HCID 23113375、化合物

HRID 2102259ノート

反応式

HRID 2102259 の反応式
[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

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 178470082HCID 178470082、化合物

生成物 1

HCID 23113375HCID 23113375、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-734388e1ec3449abbc6311f085b6585c
出典データセット
uspto-grants-2009_08
特許番号
US07576064B2

反応ノート

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