Water → HCID 14209146, 화합물

HRID 279777노트

반응식

HRID 279777 반응식
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]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 13505933HCID 13505933, 화합물

생성물 1

HCID 14209146HCID 14209146, 화합물수율 75.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eaac1cbff3774d55943b3b5b91e2ef6c
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587049

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