反応 #2446119

反応方程式

L-arginine

Tazobactam acid

acetone

→

tazobactam arginine

収率 82.0%

溶媒

water acetone

反応条件

後処理

1. 1
   その他crystallization
2. 2
   温度the suspension was cooled down to 15° C. at 0.1° C./min
3. 3
   workup.STIRRINGkept stirring at 15° C. for additional 1.5 hr
4. 4
   ろ過White fine needle crystals were filtered out
5. 5
   その他vacuum dried for 2 hours at 35° C.

実験手順

L-arginine (1.16 g) was charged to the reactor and dissolved in a mixture of deionized water-acetone (1:1, v/v, 40 mL) by mechanically stirring at 300 rpm, 30° C. over 5 min. Tazobactam acid (2.00 g) was then added to the above solution over 2 min with the observed pH change from 10.5±0.5 to 5.9±0.5. After adding 34.5 mL of acetone over 30 min at 30° C., crystallization started, then the suspension was cooled down to 15° C. at 0.1° C./min and kept stirring at 15° C. for additional 1.5 hr. White fine needle crystals were filtered out and vacuum dried for 2 hours at 35° C. to obtain 2.59 g (82% yield) of tazobactam arginine polymorph Ia.

出典