반응 #1140125

반응 방정식

(−)-tramadol

(S)-naproxen

→

(−)-tramadol (S)-naproxen

용매

isopropanol

isopropanol

반응 조건

후처리

1. 1
   기타a third of the solvent was evaporated
2. 2
   workup.WAITwas left
3. 3
   여과The resulting suspension was filtered off
4. 4
   세척the filtrate was washed with ca. 1 mL of isopropanol
5. 5
   기타dried under vacuum (10 mm Hg) at 60° C. for 24 hours

실험 절차

A solution of (−)-tramadol (0.58 g, 2.20 mmol) in 2 mL of isopropanol was added to a stirred suspension of (S)-naproxen (1.02 g, 4.43 mmol, 2 eq) in 2 mL of isopropanol at 60° C. The resulting solution was cooled to room temperature and a third of the solvent was evaporated. The solution was seeded with 5-10 mg of crystalline (−)-tramadol-(S)-naproxen (1:2) co-crystal and was left standing at room temperature for 48 hours without stirring. The resulting suspension was filtered off, the filtrate was washed with ca. 1 mL of isopropanol and dried under vacuum (10 mm Hg) at 60° C. for 24 hours to give the co-crystal (−)-tramadol-(S)-naproxen in a 1:2 ratio as a white solid (1.31 g, 81%).

출처