반응 #534967

반응 방정식

4-Fluoro-6-methyl-1-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-1,3-dihydro-2H-benzimidazol-2-one

HCl

diethyl ether

→

4-Fluoro-6-methyl-1-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-1,3-dihydro-2H-benzimidazol-2-one hydrochloride

용매

methanol

반응 조건

후처리

1. 1
   기타The solvents were evaporated
2. 2
   기타the solid triturated in diethyl ether (14.5 vol., 500 ml) for 20 min
3. 3
   기타Diethyl ether was decanted
4. 4
   기타the white solid was dried under high vacuum at 40° C. overnight
5. 5
   기타The solid was dried under high vacuum overnight at 40° C
6. 6
   기타The solid was triturated in diethyl ether (14.5 vol, 500 ml)
7. 7
   여과filtered
8. 8
   기타dried again in the oven at 40° C./high vacuum for 4 hours
9. 9
   workup.WAITat 60° C. overnight then at 80° C. for two hours

실험 절차

4-Fluoro-6-methyl-1-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-1,3-dihydro-2H-benzimidazol-2-one free base (102.73 mmol, 34.25 g, 1 wt) was suspended in methanol (10 vol. 342 ml). HCl 1M in diethyl ether (154 ml, 1.5 eq.) was added dropwise in 20 min. The slurry was magnetically stirred at ambient temp. for 3 hours. The solvents were evaporated and the solid triturated in diethyl ether (14.5 vol., 500 ml) for 20 min. Diethyl ether was decanted and the white solid was dried under high vacuum at 40° C. overnight. Residual MeOH (7% w/w by NMR) was found. The solid was dried under high vacuum overnight at 40° C. The solid was triturated in diethyl ether (14.5 vol, 500 ml), filtered and dried again in the oven at 40° C./high vacuum for 4 hours, then at 60° C. overnight then at 80° C. for two hours. 36.1 g, 95%.

출처