Reaction #82129

Reaction equation

N-[2-(3,5-di-tert-butyl-4-hydroxyphenethyl)-4,6-difluorophenyl]-N'-(1-benzyl-4-piperidyl)urea

methanesulfonic acid

→

title compound

Yield 87.0%

N-[2-(3,5-di-tert-butyl-4-hydroxyphenethyl)-4,6-difluorophenyl]-N'-(1-benzyl-4-piperidyl)urea methanesulfonate

Yield 87.0%

Solvents

ethanol

Conditions

Workup

1. 1
   workup.DISSOLUTIONto dissolve it
2. 2
   Concentrationthis solution was concentrated
3. 3
   workup.DISSOLUTIONThe concentrate was dissolved with a mixed solvent of ethyl acetate (1 ml) and diisopropylether (3 ml)
4. 4
   TemperatureThe solution was cooled to 0°-5° C.
5. 5
   FiltrationThe resultant crystals were filtered
6. 6
   Otherdried

Procedure

N-[2-(3,5-di-tert-butyl-4-hydroxyphenethyl)-4,6-difluorophenyl]-N'-(1-benzyl-4-piperidyl)urea (0.50 g) was suspended in ethanol (10 ml) and heated at 50° C. to dissolve it. To the solution was added methanesulfonic acid (56 μl) and this solution was concentrated. The concentrate was dissolved with a mixed solvent of ethyl acetate (1 ml) and diisopropylether (3 ml). The solution was cooled to 0°-5° C. and allowed to stand overnight. The resultant crystals were filtered and dried to give the title compound (0.51 g, 87%).

Source