Hydrochloric Acid → Cephradine

HRID 1197759

反応式

HRID 1197759 の反応式
[CH3:1][C:2]1[CH2:21][S:20][C@@H:5]2[C@H:6]([NH:9][C:10]([C@H:12]([NH2:19])[C:13]3[CH2:18][CH:17]=[CH:16][CH2:15][CH:14]=3)=[O:11])[C:7](=[O:8])[N:4]2[C:3]=1[C:22]([OH:24])=[O:23].CN(C)C=O.Cl>O>[CH3:1][C:2]1[CH2:21][S:20][C@@H:5]2[C@H:6]([NH:9][C:10]([C@H:12]([NH2:19])[C:13]3[CH2:18][CH:17]=[CH:16][CH2:15][CH:14]=3)=[O:11])[C:7](=[O:8])[N:4]2[C:3]=1[C:22]([OH:24])=[O:23]

参加物

4

反応物 2

HCID 313Hydrochloric Acid2 回HCID 86747480Cephradine Dimethylformamide

生成物 1

HCID 38103Cephradine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

125 g of cephradine dimethylformamide solvate (as for example produced in step a) above) were suspended in water/conc. HCl (300/12.5) at 5° to 10° C. with stirring. The pH was adjusted to 1.6 to 2.0 by addition of hydrochloric acid in order to obtain a complete solution. The solution was filtered and the residue washed with 60 ml of water. The combined filtrate was warmed to 35° to 40° C. The pH was adjusted to 2.4 to 2.8 with triethylamine whereupon precipitation started. The stirring was maintained for several minutes. The pH was then adjusted to 4.7 to 5.1 with triethylamine and the suspension was cooled to about 25° and filtered. The residue was washed with 270 g of acetone (80% v/v) to obtain the heading compound, m.p. 190° to 200° C. (decomp.).

後処理

  1. customto obtain a complete solution
  2. filtrationThe solution was filtered
  3. washthe residue washed with 60 ml of water
  4. temperatureThe combined filtrate was warmed to 35° to 40° C
  5. customThe pH was adjusted to 2.4 to 2.8 with triethylamine whereupon precipitation
  6. temperatureThe stirring was maintained for several minutes
  7. temperaturethe suspension was cooled to about 25°
  8. filtrationfiltered
  9. washThe residue was washed with 270 g of acetone (80% v/v)
  10. customto obtain the heading compound, m.p. 190° to 200° C. (decomp.)

出典と根拠

ORDレコード
ord-f41ee769477f4d07980b8ca654185518
出典データセット
uspto-grants-1994_01
特許番号
US05278157

関連ノート

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