反应详情

A stirred suspension of K2CO3 (4.15 g, 30 mol) in 100 ml of DMF was treated in one portion with thiophenol (1.65 g, 15 mol). The compound of Example 2 (3.8 g, 15 mol) was then added and the mixture heated at 110° C.±5° C. for 2 days. Water was added and the mixture extracted twice with ether. The ether extracts were washed with H2O, dried over MgSO4 and concentrated in vacuo to yield a yellow oil. Bulb to bulb distillation yielded methyl 5-phenyl-2-phenylthio-4-thiazolecarboxylate, as a yellow oil at 130°-170° C./1 mm. This oil was crystallized from etherpetroleum ether mixtures to yield 1.6 g of white crystals, methyl 5-phenyl-2-phenylthio-4-thiazolecarboxylate, m.p. 67°-70° C., yield 33%.

1. temperaturethe mixture heated at 110° C.±5° C. for 2 days
2. extractionthe mixture extracted twice with ether
3. washThe ether extracts were washed with H2O
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customto yield a yellow oil
7. distillationBulb to bulb distillation