Reaction #548959

ord-4fbe36d5628d44b490376f262fb0ccdf

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturethe mixture is heated to the boil on a water bath for 1 hour
  2. 2
    TemperatureCooling
  3. 3
    FiltrationThe precipitated crystals are filtered off
  4. 4
    Otherrecrystallized from ethanol

Procedure

1.34 g of chloropinacoline are dissolved in 15 cc of absolute ethanol. After the addition of 1.6 g of 4-methyl-1-piperazinyl-thiocarboxamide, the mixture is heated to the boil on a water bath for 1 hour. Cooling is then effected and diethyl ether is added until the mixture remains turbid. The precipitated crystals are filtered off and recrystallized from ethanol. The resulting 2-(4-methyl-1-piperazinyl)-4-tert.butyl-thiazole hydrochloride has an M.P. of 206°. The base liberated from its hydrochloride in known manner by treatment with an aqueous sodium hydroxide solution has a B.P. of 97°-99°/0.2 mm Hg.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04064244uspto-grants-1977_12