Perchloric Acid → Florfenicol butyrate

HRID 507490ノート

反応式

HRID 507490 の反応式
[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([C@@H:11]([OH:21])[C@H:12]([NH:15][C:16]([CH:18]([Cl:20])[Cl:19])=[O:17])[CH2:13][F:14])=[CH:9][CH:10]=1)(=[O:4])=[O:3].Cl(O)(=O)(=O)=[O:23]>C(OC(=O)CCC)(=O)CCC>[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([C@@H:11]([OH:21])[C@H:12]([NH:15][C:16]([CH:18]([Cl:20])[Cl:19])=[O:17])[CH2:13][F:14])=[CH:9][CH:10]=1)(=[O:4])=[O:3].[C:11]([O-:21])(=[O:23])[CH2:8][CH2:9][CH3:10]

参加物

4

反応物 2

HCID 24247Perchloric AcidHCID 114811Florfenicol

生成物 1

HCID 131727111Florfenicol butyrate

試薬・触媒・溶媒 1

HCID 7798Butyric anhydride溶媒

実験手順

225 g of florfenicol was suspended in 330 ml of butyric anhydride in one liter round bottom flask equipped with a over head stirrer and a drying tube. To this suspension was added one ml of perchloric acid, while stirring vigorously, with a pipette. A clear solution was obtained in a few minutes. Stirring was continued for another 3 hours during which the florfenicol butyrate pro-drug was crystallized. The solid product was filtered using a Buckner funnel under vacuum, and washed thoroughly with hexane. The product was finally crystallized in ethanol and the crystallized product was washed with hexane and dried to obtain around 230 g of solid florfenicol butyrate.

後処理

  1. customequipped with a over head stirrer and a drying tube
  2. customA clear solution was obtained in a few minutes
  3. stirringStirring
  4. customthe florfenicol butyrate pro-drug was crystallized
  5. filtrationThe solid product was filtered
  6. washwashed thoroughly with hexane
  7. customThe product was finally crystallized in ethanol
  8. washthe crystallized product was washed with hexane
  9. customdried

出典と根拠

ORDレコード
ord-82ea8eaf7e6f422aaaad937db2a7df1b
出典データセット
uspto-grants-2010_08
特許番号
US07786167B2

反応ノート

読み込み中…