Benzene → HCID 14230750, 화합물

HRID 621035노트

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HRID 621035 반응식
C1C=CC=CC=1.[CH3:7][O:8][C:9]([C@H:11]1[N:14]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][C:17]=2[O:24][CH3:25])[C:13](=[O:26])[C@H:12]1[N:27]1[C:31](=[O:32])[C:30]2=[CH:33][CH:34]=[CH:35][CH:36]=[C:29]2[C:28]1=[O:37])=[O:10].C1CCN2C(=NCCC2)CC1>C(OCC)(=O)C>[CH3:7][O:8][C:9]([C@@H:11]1[N:14]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][C:17]=2[O:24][CH3:25])[C:13](=[O:26])[C@H:12]1[N:27]1[C:31](=[O:32])[C:30]2=[CH:33][CH:34]=[CH:35][CH:36]=[C:29]2[C:28]1=[O:37])=[O:10]

참가 물질

5

반응물 3

HCID 241BenzeneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 54376896HCID 54376896, 화합물

생성물 1

HCID 14230750HCID 14230750, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To 200 ml of benzene are added 8.5 g of cis-1-(2,4-dimethoxybenzyl)-3-phthalimido-2-oxoazetidine-4-carboxylic acid methyl ester and 3.1 g of 1,8-diazabicyclo[5,4,0]-7-undecene, and the mixture is heated under reflux for 72 hours. To the reaction mixture, after cooling, is added 100 ml of ethyl acetate, followed by washing with 100 ml and 50 ml of 1N-HCl, and 100 ml of water in this order. To the resulting mixture is added 100 ml of chloroform and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. To the residue is added 50 ml of ethyl acetate. The resulting insolubles are collected by filtration, and washed with 30 ml of ethyl acetate to yield 6.4 g of crude product, which is recrystallized from 220 ml of ethyl acetate to yield trans-1-(2,4-dimethoxybenzyl)-3-phthalimido-2-oxoazetidine-4-carboxylic acid methyl ester, m.p. 186°-188° C.

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 72 hours
  3. temperatureTo the reaction mixture, after cooling
  4. washby washing with 100 ml and 50 ml of 1N-HCl, and 100 ml of water in this order
  5. additionTo the resulting mixture is added 100 ml of chloroform
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. additionTo the residue is added 50 ml of ethyl acetate
  9. filtrationThe resulting insolubles are collected by filtration
  10. washwashed with 30 ml of ethyl acetate
  11. customto yield 6.4 g of crude product, which
  12. customis recrystallized from 220 ml of ethyl acetate

출처 및 근거

ORD 기록
ord-80424324bcb04836a2fb76091c59ca7f
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04822790

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