Benzene → HCID 14230750、化合物

HRID 465236ノート

反応式

HRID 465236 の反応式
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]

参加物

5

反応物 3

HCID 241BenzeneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 54376896HCID 54376896、化合物

生成物 1

HCID 14230750HCID 14230750、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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 10 ml and 50 ml of 1N-HCl, and 100ml 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.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 72 hours
  3. temperatureTo the reaction mixture, after cooling
  4. washby washing with 10 ml and 50 ml of 1N-HCl, and 100ml 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

出典と根拠

ORDレコード
ord-d48a3182a21949d1b3f3f0a8935c0c5b
出典データセット
uspto-grants-1985_10
特許番号
US04550105

反応ノート

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