4-(6-Chloro-2-methylsulfanyl-pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester synthesis

Yield:932046-78-1 95%

Reaction Conditions:

with triethylamine in dichloromethane at 20; for 16 h;

Steps:

1.A

Example 1 :4-(Piperazin-1-v)l-6-(3-trifluoromethylphenyl)-pyrimidine-2-carbonitrile A [4-(6-chloro-2-methylsulfanyl-pyrimidin-4-yl)-piperazine-1-carboxylic acid ferf-butyl ester 4,6-Dichloro-2-methylsulfanylpyrimidine (1Og) was dissolved in dichloro- methane (200 ml) and triethylamine (20.6 g) was added. The mixture was stirred at room temperature and piperazine-1-carboxylic acid terf-butyl ester (9.54 g) was added in portions. The mixture was stirred at room temperature overnight. Mixture was washed with water (200ml) then brine (100ml). The organic layer was dried (MgSO₄) then evaporated under reduced pressure to afford 4-(6-chloro-2-methyl- sulfanyl-pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester (17.9 g) as a white solid. ¹H NMR (CDCI₃): δ . 6.1 1 (s, 1 H), 3.58 (m, 4H), 3.44 (m, 4H), 2.42 (s, 3H), 1.41 (s, 9H).

References:

WO2007/39470,2007,A1 Location in patent:Page/Page column 12