Sodium Bicarbonate → HCID 67742847, 화합물

HRID 655052

반응식

HRID 655052 반응식
[CH3:1][O:2][C:3]1[CH:33]=[CH:32][C:6]([CH2:7][O:8][C:9]([C:11]2[N:16]3[C:17](=[O:29])[C@@H:18]([NH:19][C:20](=[O:28])[CH2:21][C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[C@H:15]3[S:14][CH2:13][C:12]=2[CH2:30]Cl)=[O:10])=[CH:5][CH:4]=1.[SH:34][C:35]1[CH:40]=[CH:39][N:38]=[CH:37][CH:36]=1.C(=O)([O-])O.[Na+]>CN(C)C=O>[C:22]1([CH2:21][C:20]([NH:19][C@@H:18]2[C:17](=[O:29])[N:16]3[C:11]([C:9]([O:8][CH2:7][C:6]4[CH:32]=[CH:33][C:3]([O:2][CH3:1])=[CH:4][CH:5]=4)=[O:10])=[C:12]([CH2:30][S:34][C:35]4[CH:40]=[CH:39][N:38]=[CH:37][CH:36]=4)[CH2:13][S:14][C@H:15]23)=[O:28])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 10874591(4-Methoxyphenyl)methyl (6R,7R)-3-(chloromethyl)-8-oxo-7-((2-phenylacetyl)amino)-5-thia-1-azabicyclo(4.2.0)oct-2-ene-2-carboxylateHCID 178418431pyridine-4-thiol

생성물 1

HCID 67742847HCID 67742847, 화합물수율 93.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred and ice cold solution of 7β-phenylacetamido-3-chloromethyl-3-cephem-4-carboxylic acid p-methoxybenzyl ester (1) (4.87 g; 10 mMol.) and 4-mercaptopyridine (1.45 g; 1.3 Eq.) in N,N-dimethylformamide (15 ml) is added sodium hydrogen carbonate (1.09 g; 1.3 Eq.), and the mixture is stirred at room temperature for 1 hour. The reaction mixture is diluted with ice water and separating solidis collected by filtration, dissolved in ethyl acetate, washed with water, dried, and concentrated under reduced pressure. The residue is washed with ether to give p-methoxybenzyl 7β-phenylacetamido-3-(4-pyridyl)thiomethyl-3-cephem-4-carboxylate (2) (5.25 g).

후처리

  1. stirringthe mixture is stirred at room temperature for 1 hour
  2. customseparating solidis
  3. filtrationcollected by filtration
  4. dissolutiondissolved in ethyl acetate
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. washThe residue is washed with ether

출처 및 근거

ORD 기록
ord-0f834af4318a40a9b90f1c12f6e11c4a
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05134138

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