Water → Tert-butyl 7-amino-3-methoxymethyl-3-cephem-4-carboxylate

HRID 1463090노트

반응식

HRID 1463090 반응식
S(C1C=CC(C)=CC=1)(O)(=O)=O.[NH2:12][CH:13]1[C:30](=[O:31])[N:15]2[C:16]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])=[C:17]([CH2:20][O:21][CH3:22])[CH2:18][S:19][C@H:14]12.O.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[NH2:12][CH:13]1[C:30](=[O:31])[N:15]2[C:16]([C:23]([O:25][C:26]([CH3:27])([CH3:28])[CH3:29])=[O:24])=[C:17]([CH2:20][O:21][CH3:22])[CH2:18][S:19][C@H:14]12

참가 물질

5

반응물 3

HCID 962WaterHCID 516892Sodium BicarbonateHCID 131713144Tert-butyl 7-amino-3-methoxymethyl-3-cephem-4-carboxylate tosylate

생성물 1

HCID 67712488Tert-butyl 7-amino-3-methoxymethyl-3-cephem-4-carboxylate수율 68.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of tert-butyl 7-amino-3-methoxymethyl-3-cephem-4-carboxylate tosylate (13.1 g) in methylene chloride (200 ml) was added water (100 ml), followed by adjusting to pH about 6 with an aqueous solution of sodium bicarbonate. After separating out the methylene chloride layer, the remaining aqueous solution was extracted with methylene chloride (50 ml). The combined methylene chloride solution was washed with an aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate and then treated with an activated charcoal, followed by evaporation under reduced pressure to give tert-butyl 7-amino-3-methoxymethyl-3-cephem-4-carboxylate (5.7 g).

후처리

  1. customAfter separating out the methylene chloride layer
  2. extractionthe remaining aqueous solution was extracted with methylene chloride (50 ml)
  3. washThe combined methylene chloride solution was washed with an aqueous solution of sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. additiontreated with an activated charcoal
  6. customfollowed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-3bb8687ebcab44d0a254a8549e95a934
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04462999

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