Water → Tert-butyl 2-(2-oxo-3-benzylimidazolidinyl)acetate

HRID 23559

反応式

HRID 23559 の反応式
[CH2:1]([N:8]1[CH2:12][CH2:11][NH:10][C:9]1=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(C)([O-])C.[Li+].Br[CH2:21][C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23].O>CN(C=O)C>[O:13]=[C:9]1[N:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:12][CH2:11][N:10]1[CH2:21][C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23]

参加物

6

反応物 4

HCID 962WaterHCID 79177tert-Butyl bromoacetateHCID 2314031-Benzylimidazolidin-2-oneHCID 236647642-Propanol, 2-methyl-, lithium salt (1:1)

生成物 1

HCID 22574612Tert-butyl 2-(2-oxo-3-benzylimidazolidinyl)acetate収率 87.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-benzylimidazolidin-2-one (3.5 g, 19.9 mmol) in DMF (50 ml) at 0° C. were added lithium tert-butoxide (1.9 g, 23.8 mmol) and tert-butyl bromoacetate (3.2 ml, 21.8 mmol). After stirring the mixture at room temperature overnight, the reaction mixture was poured into water (100 ml) and the mixture was extracted with ethyl acetate. The organic phase was washed with water, 10% aqueous citric acid solution, saturated aqueous sodium hydrogen carbonate solution and brine. The organic solution was dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The crystalline residue was washed with n-hexane, and dried to give tert-butyl 2-(2-oxo-3-benzylimidazolidinyl)acetate (5.08 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic phase was washed with water, 10% aqueous citric acid solution, saturated aqueous sodium hydrogen carbonate solution and brine
  3. dry with materialThe organic solution was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. washThe crystalline residue was washed with n-hexane
  7. customdried

出典と根拠

ORDレコード
ord-2c8c23d821ec48c48d63b3ece07d1294
出典データセット
uspto-grants-2005_02
特許番号
US06852744B2

関連ノート

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