Sodium Bicarbonate → HCID 88770327, 화합물

HRID 127098노트

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HRID 127098 반응식
C(O[CH2:5][C:6]1[CH2:7][S:8][C@@H:9]2[CH:16]([NH:17][C:18](=[O:26])[CH2:19][C:20]3[S:24][C:23]([NH2:25])=[N:22][CH:21]=3)[C:15](=[O:27])[N:10]2[C:11]=1[C:12]([OH:14])=[O:13])(=O)C.[CH3:28][N:29]1[C:33]([S-:34])=[N:32][N:31]=[N:30]1.[K+].C(=O)(O)[O-].[Na+]>P([O-])([O-])([O-])=O>[CH3:28][N:29]1[C:33]([S:34][CH2:5][C:6]2[CH2:7][S:8][C@@H:9]3[CH:16]([NH:17][C:18](=[O:26])[CH2:19][C:20]4[S:24][C:23]([NH2:25])=[N:22][CH:21]=4)[C:15](=[O:27])[N:10]3[C:11]=2[C:12]([OH:14])=[O:13])=[N:32][N:31]=[N:30]1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 23681836Potassium 1-methyl-1H-tetrazole-5-thiolateHCID 88769766HCID 88769766, 화합물

생성물 1

HCID 88770327HCID 88770327, 화합물수율 49.4%

시약·촉매·용매 1

HCID 1061Phosphate용매

실험 절차

A solution of 3-acetoxymethyl-7-(2-aminothiazol-5-yl)acetamido-3-cephem-4-carboxylic acid (2 g.) and potassium 1-methyl-1H-tetrazole-5-thiolate (0.7 g.) in pH 6.4 phosphate buffer (50 ml.) was stirred for 4 hours with continuous introduction of nitrogen gas while the reaction mixture was kept to pH 6.4 to 7 with sodium bicarbonate. After the reaction, the reaction mixture was cooled and then filtered. The filtrate was adjusted to pH 2.5 with diluted hydrochloric acid under ice-cooling, and the precipitates were collected by filtration and then purified similarly as that of Example 6 to give light brown powder of 3-(1-methyl-1H-tetrazol-5-yl)thiomethyl-7-(2-aminothiazol-5-yl)acetamido-3-cephem-4-carboxylic acid (1.05 g.).

후처리

  1. customAfter the reaction
  2. temperaturethe reaction mixture was cooled
  3. filtrationfiltered
  4. temperaturecooling
  5. filtrationthe precipitates were collected by filtration
  6. custompurified similarly as that of Example 6

출처 및 근거

ORD 기록
ord-a1f95acbfa2e4c048eda6d4b10bb73c4
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254260

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