反応 #64272

反応方程式

loracarbef monohydrate

loracarbef monohydrate

Ethyl p-hydroxybenzoate

HCl

→

loracarbef

収率 98.2%

溶媒

ethanol

反応条件

後処理

1. 1
   その他precipitation
2. 2
   その他resulting in white crystals
3. 3
   ろ過filtered
4. 4
   洗浄washed with H2O
5. 5
   その他dried under vacuum at 40° C

実験手順

The pH of aqueous loracarbef monohydrate mother liquor (1000 ml, having 9.23 mg/ml of loracarbef monohydrate) was adjusted to 3.6 with HCl. Ethyl p-hydroxybenzoate (ethyl paraben) (4.52g) in ethanol (36 ml) was added dropwise over 15 minutes. After approximately 5 minutes, precipitation occurred, resulting in white crystals. The mixture was stirred overnight (15 hrs) at room temperature, filtered, washed with H2O, and dried under vacuum at 40° C. The yield was 11.72 g having a potency of 73.5% as loracarbef, and the theoretical yield was 8.78 g as loracarbef, resulting in a percent yield of 98.2%. The loracarbef:ethyl paraben exhibited the following X-ray powder diffraction pattern:

出典