C(NC(C)C)(C)C.C([Li])CCC.[CH3:13][C:14]1[CH:19]=[CH:18][N:17]=[C:16]([S:20][CH3:21])[N:15]=1.[Cl:22][C:23]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:24]=1[C:25](N(OC)C)=[O:26].[NH4+].[Cl-]>C(Cl)Cl.C1COCC1>[Cl:22][C:23]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:24]=1[C:25](=[O:26])[CH2:13][C:14]1[CH:19]=[CH:18][N:17]=[C:16]([S:20][CH3:21])[N:15]=1To the solution of 85 mL of diisopropylamine (Fluka 38300) and 2.5 L of THF at −75° C. under Argon is added 370 mL (0.55 Mol) of butyl lithium (BuLi; 1.6N in hexanes; Fluka 20160) within 1 h. To this is added 71 g (0.5 Mol) of 4-methyl-2-methylsulfanyl-pyrimidine in 250 mL of CH2Cl2 at −75° C. within 30 min. After this, a solution of 118 g (0.5 Mol) of 2,4dichloro-N-methoxy-N-methyl-benzamide in 250 mL of CH2Cl2 at −75° C. within 30 min followed by letting the mixture warn up to rt. After completion, the reaction mixture is poured onto 7 L of NH4Cl satd. and extracted with ethyl acetate. The combined organic layers are washed with brine, dried and evaporated. The crude product is suspended in hexanes. After filtering off and drying 1-(2,4-dichloro-phenyl)-2-(2-methylsulfanyl-pyrimidin-4-yl)-ethanone is obtained as yellow crystals. Title compound: m.p.: 105-107° C.; ES-MS: 313.0/314.9 [M+H]+.
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