반응 #1140126

ord-66ec71c51e90449bbcc928a39446ce0f

반응 방정식

COc1ccc2cc([C@@H](C)C(=O)O)ccc2c1
(R)-naproxen
COc1cccc([C@@]2(O)CCCC[C@@H]2CN(C)C)c1
(+)-tramadol
COc1ccc2cc([C@@H](C)C(=O)O)ccc2c1.COc1cccc([C@@]2(O)CCCC[C@@H]2CN(C)C)c1
(+)-tramadol (R)-naproxen

시약

없음

반응 조건

온도
-197°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the solvent was evaporated under vacuum
  2. 2
    workup.STIRRINGstirred for 7 days at room temperature
  3. 3
    여과The resulting suspension was filtered off
  4. 4
    세척The filtrate was washed with 5 mL of diisopropyl ether
  5. 5
    기타dried under vacuum at 40° C. (10 mm Hg) for 16 hours

실험 절차

A solution of (R)-naproxen (751 mg, 3.26 mmol) in 4 mL of methanol was added to a solution of (+)-tramadol (430 mg, 1.63 mmol) in 1 mL of methanol. The mixture was stirred for 30 minutes and the solvent was evaporated under vacuum rendering an oil, which solidified by cooling to −197° C. The resulting solid was suspended in 10 mL of diisopropyl ether and stirred for 7 days at room temperature. The resulting suspension was filtered off. The filtrate was washed with 5 mL of diisopropyl ether and dried under vacuum at 40° C. (10 mm Hg) for 16 hours to give a co-crystal of (+)-tramadol-(R)-naproxen in a 1:2 ratio as a crystalline white solid (620 mg, 53%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09393220B2uspto-grants-2016_07