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Sodium hydride → 1-(alpha-Benzyloxycarbonyl-4-benzyloxybenzyl)-3-(2-phenylacetamido)-2-azetidinone

HRID 1706514
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HRID 1706514 반응식
[C:1]1([CH2:7][C:8]([NH:10][CH:11]2[CH2:14][NH:13][C:12]2=[O:15])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[CH:17]([C:28]1[CH:33]=[CH:32][C:31]([O:34][CH2:35][C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[CH:30][CH:29]=1)[C:18]([O:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:19].[H-].[Na+]>CN(C)C=O>[CH2:21]([O:20][C:18]([CH:17]([N:13]1[CH2:14][CH:11]([NH:10][C:8](=[O:9])[CH2:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:12]1=[O:15])[C:28]1[CH:33]=[CH:32][C:31]([O:34][CH2:35][C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[CH:30][CH:29]=1)=[O:19])[C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 132120483-[(Phenylacetyl)amino]-2-azetidinoneHCID 20334848Benzyl 2-bromo-2-(4-benzyloxyphenyl)acetate

생성물 1

HCID 536735461-(alpha-Benzyloxycarbonyl-4-benzyloxybenzyl)-3-(2-phenylacetamido)-2-azetidinone

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3-(2-Phenylacetamido)-2-azetidinone (750 mg.) and benzyl 2-bromo-2-(4-benzyloxyphenyl)acetate (1.51 g.) was added to anhydrous N,N-dimethylformamide (10 ml.), and disdolved in it by warming for a while. The solution was cooled in an ice-water bath, and to the solution was added all at once sodium hydride (50% oily) (178 mg.) under stirring. After removing the cooling bath, the reaction mixture was stirred for 30 minutes to which ethyl acetate was added. The reaction mixture was filtered and the filtrate was washed with water, 2% hydrochloric acid and water respectively, and then dried over anhydrous magnesium sulfate. The solution was concentrated under reduced pressure to give an oily material (1.98 g.), which was subjected to column chromatography using silica.gel (40 g.). The fractions, eluted with a mixture of benzene and chloroform were subjected to thin layer chromatography using silica.gel, and the thin layer was developed with a mixture of chloroform and acetone to give two isomers of 1-(α-benzyloxycarbonyl-4-benzyloxybenzyl)-3-(2-phenylacetamido)-2-azetidinone. The isomer A was recrystallized from a mixture of chloroform and ether. Yield: 90 mg. Mp: 129° to 130° C. (dec.). The isomer B is oily material. Yield: 120 mg. The isomer A (90 mg.) obtained above was dissolved in methanol (7 ml.), and to the solution was added 10% palladium carbon (30 mg.). The mixture was reacted in hydrogen atmosphere at ordinary temperature and ordinary atm. until the absorption of hydrogen gas was completed. The catalyst was filtered off from the fraction mixture, and the filtrate was concentrated under reduced pressure. The residue obtained was crystallized from a mixture of ethyl acetate and ether to give crystals of 3-(2-phenylacetamido)lactacillanic acid. The product was identified by comparing an I.R. absorption spectrum and a N.M.R. absorption spectrum and a melting point with an authentic sample synthesized by another method from 3-aminolactacillanic acid.

후처리

  1. temperatureby warming for a while
  2. temperatureThe solution was cooled in an ice-water bath
  3. customAfter removing the cooling bath
  4. stirringthe reaction mixture was stirred for 30 minutes to which ethyl acetate
  5. additionwas added
  6. filtrationThe reaction mixture was filtered
  7. washthe filtrate was washed with water, 2% hydrochloric acid and water respectively
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationThe solution was concentrated under reduced pressure
  10. customto give an oily material (1.98 g.), which
  11. washThe fractions, eluted with a mixture of benzene and chloroform
  12. additiongel, and the thin layer was developed with a mixture of chloroform and acetone

출처 및 근거

ORD 기록
ord-a8bed5f5bc1840b1873bdd4fad2742bc
출처 데이터셋
uspto-grants-1980_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04207234

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