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With 3-chloro-benzenecarboperoxoic acid; In chloroform;
Reference Synthesis Example 3 Synthesis of 4-chloro-6-methyl-2-(methylsulfonyl)pyrimidine (Compound III-7) 4-Chloro-6-methyl-2-(methylthio)pyrimidine (Compound IV-7) (2.0 g, 0.0114 mol) was dissolved in chloroform, m-chloroperbenzoic acid (5.64 g, (purity ca. 70%), 0.0114*2.0 mol) was added thereto and the solution was stirred for about 2 hours at room temperature. The reaction solution was partitioned between chloroform and saturated aqueous sodium hydrogen carbonate to separate an organic phase, which was then washed with saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, concentrated, and thereafter, purified on silica gel column to obtain the compound (III-7). Yield: 2.25 g (95%). m.p. 67 to 70 C. 1 H-NMR (60 MHz, CDCl3, delta): 2.63(3H,s), 3.30(3H,s), 7.38 (1H,s).
With 3-chloro-benzenecarboperoxoic acid; In chloroform;
(1) Synthesis of an intermediate, 4-chloro-6-methyl-2-(methylsulfonyl)pyrimidine (Compound No. VIII-4) 4-Chloro-6-methyl-2-(methylthio)pyrimidine (2.0 g, 0.0114 mol) (Compound No. VII-4) was dissolved in chloroform, and m-CPBA (5.64 g (purity ca.70%), 0.0114*2.0 mol) was added thereto, and then the resulting solution was allowed to react for about 2 hours at room temperature. The reaction solution was partitioned between chloroform and aqueous saturated sodium hydrogen carbonate to separate an organic phase. The organic phase was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated, thereafter the residue was purified on a silica gel column to obtain the Compound No. VIII-4.
With sodium hypochlorite; chlorine; In hydrogenchloride; water;
EXAMPLE 10 STR124 1.9 l of sodium hypochlorite (about 150 g of active chlorine per liter) were added slowly to a solution of 175 g (1 mole) of 2-methylmercapto-4-methyl-6-chloropyrimidine in 375 ml of concentrated hydrochloric acid and 375 ml of water at 5 C. The product which had precipitated was then filtered off and rinsed with water. This gave 170 g (82% of theory) of 2-methylsulfonyl-4-methyl-6-chloropyrimidine in the formn of colorless crystals of melting point 72 C. STR125
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