Water → HCID 14209146、化合物

HRID 279777ノート

反応式

HRID 279777 の反応式
C([O:3][C:4]([CH:6]1[CH2:9][C:8](=[O:10])[N:7]1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][C:13]=1[O:20][CH3:21])=[O:5])C.[OH-].[Na+].O>C(O)C>[CH3:21][O:20][C:13]1[CH:14]=[C:15]([O:18][CH3:19])[CH:16]=[CH:17][C:12]=1[CH2:11][N:7]1[C:8](=[O:10])[CH2:9][CH:6]1[C:4]([OH:5])=[O:3]

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 13505933HCID 13505933、化合物

生成物 1

HCID 14209146HCID 14209146、化合物収率 75.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 5.80 g (0.020 mole) of ethyl-[1-(2,4-dimethoxy-benzyl)-4-oxo-2-azetidine-carboxylate] in 25 ml of ethanol a solution of 0.88 g (0.022 mole) of sodium hydroxide and 60 ml of water is added. The reaction solution is stirred for 2 hours and extracted three times with 20 ml of ether each. The aqueous layer is acidified to pH 2 with concentrated aqueous hydrochloric acid and extracted three times with 20 ml of dichloromethane each. The united organic solutions are dried over anhydrous magnesium sulfate, filtered and from the filtrate the dichloromethane is distilled off. The residue is treated with ether, the yellowish-white crystalline product is filtered off and recrystallized from benzene. Thus 4.0 g of 1-(2,4-dimethoxy-benzyl)-4-oxo-2-azetidine-carboxylic acid are obtained. Yield: 75.4%. M.p.: 124°-125° C.

後処理

  1. extractionextracted three times with 20 ml of ether each
  2. extractionextracted three times with 20 ml of dichloromethane each
  3. dry with materialThe united organic solutions are dried over anhydrous magnesium sulfate
  4. filtrationfiltered and from the filtrate the dichloromethane
  5. distillationis distilled off
  6. additionThe residue is treated with ether
  7. filtrationthe yellowish-white crystalline product is filtered off
  8. customrecrystallized from benzene

出典と根拠

ORDレコード
ord-eaac1cbff3774d55943b3b5b91e2ef6c
出典データセット
uspto-grants-1986_05
特許番号
US04587049

反応ノート

読み込み中…