Acetone → cefpodoxime sodium

HRID 989420ノート

反応式

HRID 989420 の反応式
C([O-])(=O)C.[Na+:5].[CH3:6][O:7][CH2:8][C:9]1[CH2:30][S:29][C@@H:12]2[C@H:13]([NH:16][C:17](/[C:19](/[C:23]3[N:27]=[C:26]([NH2:28])[S:25][CH:24]=3)=[N:20]\[O:21][CH3:22])=[O:18])[C:14](=[O:15])[N:11]2[C:10]=1[C:31]([OH:33])=[O:32].CN(C)C(=O)C.CC(C)=O>O.CO>[CH3:6][O:7][CH2:8][C:9]1[CH2:30][S:29][C@@H:12]2[C@H:13]([NH:16][C:17](/[C:19](/[C:23]3[N:27]=[C:26]([NH2:28])[S:25][CH:24]=3)=[N:20]\[O:21][CH3:22])=[O:18])[C:14](=[O:15])[N:11]2[C:10]=1[C:31]([O-:33])=[O:32].[Na+:5]

参加物

7

反応物 4

HCID 180AcetoneHCID 31374DimethylacetamideHCID 517045Sodium AcetateHCID 6335986Cefpodoxime

生成物 1

HCID 23669317cefpodoxime sodium収率 96%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

1.01 g of sodium acetate was dissolved in a mixture of 1 ml of water and 5 ml of methanol, and 5.0 g of cefpodoxime was added thereto, followed by addition of 15 ml of N,N-dimethylacetamide. The mixture was stirred at room temperature for 30 minutes and then, 100 ml of acetone was added thereto. The solution was stirred for 20 minutes and filtered. The filtered solid was washed with 50 ml of acetone and then with 30 ml of isopropyl ether, and vacuum-dried at room temperature to give 5.04 g of pale yellow cefpodoxime sodium salt (yield: 96%).

後処理

  1. additionwas added
  2. stirringThe solution was stirred for 20 minutes
  3. filtrationfiltered
  4. washThe filtered solid was washed with 50 ml of acetone
  5. dry with materialwith 30 ml of isopropyl ether, and vacuum-dried at room temperature

出典と根拠

ORDレコード
ord-bc90c490d620440cab7eef9ecb548d4b
出典データセット
uspto-grants-2003_10
特許番号
US06639068B1

反応ノート

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