반응 #543097

ord-622e3e675a384c18b597715b8e805b30

반응 방정식

CCCc1nn(C)c2c(=O)[nH]c(-c3cc(S(=O)(=O)N4CCN(C)CC4)ccc3OCC)nc12.O=C(O)CC(O)(CC(=O)O)C(=O)O
Sildenafil citrate
Cl
HCl
CO
methanol
→
CCCc1nn(C)c2c(=O)nc(-c3cc(S(=O)(=O)N4CCN(C)CC4)ccc3OCC)[nH]c12.Cl
Sildenafil HCl

반응물

CCCc1nn(C)c2c(=O)[nH]c(-c3cc(S(=O)(=O)N4CCN(C)CC4)ccc3OCC)nc12.O=C(O)CC(O)(CC(=O)O)C(=O)O
Sildenafil citrate
Cl
HCl
CO
methanol

시약

없음

용매

CCO
ethanol

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타reacted at 50° C. for 10 mins
  2. 2
    workup.WAITfor incubating over night
  3. 3
    기타crystallization
  4. 4
    여과Then, the crystal is filtrated

실험 절차

Sildenafil citrate (9.5 g) is dissolved in a mixture of ethanol (10 mL) and HCl (1N, 60 mL), then reacted at 50° C. for 10 mins. Under room temperature, the methanol is added for incubating over night and crystallization. Then, the crystal is filtrated to obtain precipitate of Sildenafil HCl (6.4 g) for use.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08497370B2uspto-grants-2013_07