반응 #534969

반응 방정식

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

acetonitrile

Methanesulfonic acid

→

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

용매

n-propanol

반응 조건

후처리

1. 1
   기타giving a white slurry
2. 2
   온도The contents of the flask were heated
3. 3
   workup.DISSOLUTIONdissolved
4. 4
   기타a white precipitate formed
5. 5
   온도After cooling to ambient temperature
6. 6
   기타the solid was isolated by vacuum filtration
7. 7
   세척washed with acetonitrile (10 vol. 5 ml)
8. 8
   기타The white solid was dried under high vacuum at 60° C. for 25 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 (1.499 mmol, 500 mg, 1 wt) was weighed into a 250 ml round bottomed flask, acetonitrile (95 vol., 47.5 ml) and n-propanol (80 vol., 40 ml) were added, giving a white slurry. Methanesulfonic acid (1 eq, 1.499 mmol, 97 □l) was pipetted into the flask. The contents of the flask were heated using a hot air gun—the slurry dissolved and a white precipitate formed. The precipitate was magnetically stirred at 35° C. for four days under nitrogen. After cooling to ambient temperature, the solid was isolated by vacuum filtration and washed with acetonitrile (10 vol. 5 ml). The white solid was dried under high vacuum at 60° C. for 25 hours. 561 mg, 87%, white solid.

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