反応 #64273

反応方程式

triethylamine

loracarbef

ethyl paraben

hydrochloric acid

→

Loracarbef DMF

収率 85.3%

溶媒

DMF

H2O

反応条件

後処理

1. 1
   その他to obtain a clear solution
2. 2
   その他the crystallization of the titled product
3. 3
   ろ過filtered
4. 4
   洗浄washed with a solution of 10:1/DMF
5. 5
   乾燥H2O, and dried under a vacuum at 40° C

実験手順

To a mixture of loracarbef: ethyl paraben (1.34 g, 65.5% potency as loracarbef) in 18 ml of DMF and 1.8 ml of H2O was added concentrated hydrochloric acid sufficient to obtain a clear solution. The pH of the solution was slowly raised to 6.9 with triethylamine, and the crystallization of the titled product occurred quickly. The mixture was stirred for 1 hour at room temperature, filtered, washed with a solution of 10:1/DMF:H2O, and dried under a vacuum at 40° C. HPLC analysis indicated that no ethyl paraben was present. The actual yield was 1.01 g, 73.9% potency as loracarbef, the theoretical yield was 0.87 g as loracarbef, and the percent yield was 85.3%.

出典