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

HRID 1463090ノート

反応式

HRID 1463090 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3bb8687ebcab44d0a254a8549e95a934
出典データセット
uspto-grants-1984_07
特許番号
US04462999

反応ノート

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