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Triethylamine → HCID 131711626, 화합물

HRID 28016
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HRID 28016 반응식
[S:1]([N:11]1[C:15](=[O:16])[C:14]2=[CH:17][CH:18]=[CH:19][CH:20]=[C:13]2[C:12]1=[O:21])([C:4]1[CH:10]=[CH:9][C:7]([CH3:8])=[CH:6][CH:5]=1)(=[O:3])=[O:2].C(N(CC)CC)C.[Na+:29].[S:30]1[CH:34]=[CH:33][CH:32]=[C:31]1[CH2:35][C:36]([NH:38][C@@H:39]1[C:51](=[O:52])[N:41]2[C:42]([C:48]([O-:50])=[O:49])=[C:43]([CH2:46][OH:47])[CH2:44][S:45][C@H:40]12)=[O:37]>CN(C)C=O.O>[Na+:29].[S:30]1[CH:34]=[CH:33][CH:32]=[C:31]1[CH2:35][C:36]([NH:38][C@@H:39]1[C:51](=[O:52])[N:41]2[C:42]([C:48]([O-:50])=[O:49])=[C:43]([CH2:46][O:47][C:15](=[O:16])[C:14]3[CH:17]=[CH:18][CH:19]=[CH:20][C:13]=3[C:12](=[O:21])[NH:11][S:1]([C:4]3[CH:10]=[CH:9][C:7]([CH3:8])=[CH:6][CH:5]=3)(=[O:3])=[O:2])[CH2:44][S:45][C@H:40]12)=[O:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 2141332-((4-Methylphenyl)sulfonyl)-1H-isoindole-1,3(2H)-dioneHCID 23695995Desacetylcephalothin sodium

생성물 1

HCID 131711626HCID 131711626, 화합물수율 58.5%

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

실험 절차

In N,N-dimethylformamide (40 ml) is dissolved in 7β-(2-thienylacetamido)-3-hydroxymethyl-3-cephem-4-carboxylic acid sodium salt (3.8 g), followed by the addition of N-tosylphthalimide (4.0 g) and triethylamine (2.0 ml) in that order. The mixture is stirred at room temperature for 4 hours. The reaction mixture is poured in water (100 ml) and rinsed with ethyl acetate. The aqueous layer is adjusted to pH 2.0 with dilute phosphoric acid and extracted with ethyl acetate. The extract is dried and, then, a solution of sodium 2-ethylhexanoate in isopropyl alcohol is added. By this procedure is obtained 7β-(2-thienylacetamido)-3-[2-(N-tosylcarbamoyl) benzoyloxy]methyl-3-cephem-4-carboxylic acid sodium salt (4.0 g).

후처리

  1. washrinsed with ethyl acetate
  2. extractionextracted with ethyl acetate
  3. customThe extract is dried
  4. additiona solution of sodium 2-ethylhexanoate in isopropyl alcohol is added

출처 및 근거

ORD 기록
ord-5bf41c9eee674cbeb5ae848a5e81ec75
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04224441

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