Ethanol → HCID 14209149、化合物

HRID 279779ノート

反応式

HRID 279779 の反応式
[CH3:1][O:2][C:3]1[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[C:9](=[O:10])[CH2:8][CH:7]1[CH2:11][C:12]([O:14]CC)=[O:13].C(O)C.[OH-].[Na+]>O>[CH3:1][O:2][C:3]1[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[C:9](=[O:10])[CH2:8][CH:7]1[CH2:11][C:12]([OH:14])=[O:13]

参加物

5

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 54369044HCID 54369044、化合物

生成物 1

HCID 14209149HCID 14209149、化合物収率 96.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 0.31 g (1 millimole) of ethyl [1-(2,4-dimethoxy-benzyl)-4-oxo-2-azetidinyl]-acetate and 4 ml of ethanol a solution of 0.04 g (1 millimole) of sodium hydroxide and 6 ml of water are added. The reaction mixture is stirred at room temperature for 2 hours. The solution is extracted three times with 3 ml of dichloromethane each. The aqueous layer is acidified with concentrated aqueous hydrochloric acid to pH 2 and extracted three times with 3 ml of dichloromethane each. The united organic layers are dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated. The residue is crystallized from benzene. Thus 0.27 g of the desired compound are obtained, yield: 88%, M.p.: 112° C.

後処理

  1. extractionThe solution is extracted three times with 3 ml of dichloromethane each
  2. extractionextracted three times with 3 ml of dichloromethane each
  3. dry with materialThe united organic layers are dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customthe filtrate is evaporated
  6. customThe residue is crystallized from benzene

出典と根拠

ORDレコード
ord-ee76ee87ee8744208d54f8e3234bc2cf
出典データセット
uspto-grants-1986_05
特許番号
US04587049

反応ノート

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