Hydrochloric Acid → HCID 131715952, 화합물

HRID 1762688노트

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HRID 1762688 반응식
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:7](=[N:28][O:29][CH3:30])[C:8]([NH:10][C@@H:11]2[C:26](=[O:27])[N:13]3[C:14]([C:23]([O-:25])=[O:24])=[C:15]([CH2:18]OC(=O)C)[CH2:16][S:17][C@H:12]23)=[O:9])[N:6]=1.[Na+].[I-].[Na+].[O:34]1[CH:38]=[CH:37][N:36]=[C:35]1[C:39]1[CH:44]=[CH:43][N:42]=[CH:41][CH:40]=1.Cl>CC(C)=O.C(#N)C>[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:7](=[N:28][O:29][CH3:30])[C:8]([NH:10][C@@H:11]2[C:26](=[O:27])[N:13]3[C:14]([C:23]([O-:25])=[O:24])=[C:15]([CH2:18][N+:42]4[CH:41]=[CH:40][C:39]([C:35]5[O:34][CH:38]=[CH:37][N:36]=5)=[CH:44][CH:43]=4)[CH2:16][S:17][C@H:12]23)=[O:9])[N:6]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 3752778Pyridine, 4-(2-oxazolyl)-HCID 23675341HCID 23675341, 화합물

생성물 1

HCID 131715952HCID 131715952, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 6342Acetonitrile용매

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온도
80 °C

실험 절차

0.75 g of sodium 7β-[2-(2-aminothiazol-4-yl)-2-methoxyiminoacetamido]-3-acetoxymethyl-3-cephem-4-carboxylate (hereinafter referred to Compound 1), 2.25 g of sodium iodide and 0.51 g of 4-(oxazol-2-yl)-pyridine were added to a mixture of 0.4 ml of 4 N hydrochloric acid and 1.2 ml of acetonitrile, followed by stirring at 80° C. for 1 hour. After allowing the mixture to cool, the reaction mixture was poured into acetone, and the precipitate formed was separated by filtration and washed with acetone. The resulting crude powder was dissolved in water, and the solution was subjected to column chromatography of Diaion HP-20 (trade name of Mitsubishi Chemical Industries, Ltd.). The column was developed with a mixture of water-tetrahydrofuran (93:7 by volume). The eluate was further subjected to reversed phase high performance liquid chromatography (column packing: Develosil, trade name of Nomura Chemical Co., Ltd.) and developed with a mixture of water-acetonitrile (89:11 by volume) to obtain the titled compound. Melting point: 160°-170° C. (decomposition).

후처리

  1. temperatureto cool
  2. customthe precipitate formed
  3. customwas separated by filtration
  4. washwashed with acetone
  5. dissolutionThe resulting crude powder was dissolved in water
  6. additionThe column was developed with a mixture of water-tetrahydrofuran (93:7 by volume)
  7. additiondeveloped with a mixture of water-acetonitrile (89:11 by volume)

출처 및 근거

ORD 기록
ord-52debf76abc64562b3357f55012ae191
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04833242

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