Trifluoromethanesulfonic acid → 1-Benzoyl-5,5-dimethylimidazolidin-2-one

HRID 2411181ノート

反応式

HRID 2411181 の反応式
[C:1]([N:9]1[C:13]([CH3:15])([CH3:14])[CH2:12][N:11](CC2C=CC(OC)=CC=2)[C:10]1=[O:25])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.FC(F)(F)S(O)(=O)=O.C(=O)([O-])O.[Na+]>ClCCl>[C:1]([N:9]1[C:13]([CH3:14])([CH3:15])[CH2:12][NH:11][C:10]1=[O:25])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 62406Trifluoromethanesulfonic acidHCID 516892Sodium BicarbonateHCID 712524583-Benzoyl-1-(4-methoxybenzyl)-4,4-dimethylimidazolidin-2-one

生成物 1

HCID 712521131-Benzoyl-5,5-dimethylimidazolidin-2-one収率 45.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-Benzoyl-1-(4-methoxybenzyl)-4,4-dimethylimidazolidin-2-one (500 mg) described in Preparation Example 57 was dissolved in dichloromethane (5 mL), trifluoromethanesulfonic acid (0.39 mL) was added, and the mixture was stirred at room temperature for 3 hr. To the reaction mixture was added 5% aqueous sodium hydrogen carbonate solution, the solvent was evaporated, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and the solvent was evaporated. The obtained residue was purified by column chromatography (hexane:ethyl acetate) to give the title compound (146 mg).

後処理

  1. customthe solvent was evaporated
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. customthe solvent was evaporated
  5. customThe obtained residue was purified by column chromatography (hexane:ethyl acetate)

出典と根拠

ORDレコード
ord-73656e08363748a8839c80050d0edbc5
出典データセット
uspto-grants-2014_08
特許番号
US08816079B2

反応ノート

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