反应详情

A mixture of p-chlorophenoxymethyl chloride (6 mmol) and the potassium salt of 5-chloropyrimidine-2-thione (5 mmol) in 1,2-dimethoxyethane (25 ml) was stirred at room temperature for 10 h, the solvent distilled off at reduced pressure, the residue extracted with chloroform (70 ml), the chloroform (70 ml), the chloroform solution washed with 1 M NaOH (2×10 ml) and water (10 ml), and the dried (MgSO4) solution evaporated. The residual sulfide was recrystallized from iPrOH; yield 70%, m.p. 120° C. 1H NMR (DMSO-d6): δ5.90 (SCH2), 6.98 and 7.31 (Ph), 8.78 (H-4, H-6).

1. distillationthe solvent distilled off at reduced pressure
2. extractionthe residue extracted with chloroform (70 ml)
3. washthe chloroform (70 ml), the chloroform solution washed with 1 M NaOH (2×10 ml) and water (10 ml)
4. dry with materialthe dried (MgSO4) solution
5. customevaporated
6. customThe residual sulfide was recrystallized from iPrOH