Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 3-Cyanophenol | HCID 13394 | — |
| Reactant | Ethyl 4-chloro-1,3-thiazole-5-carboxylate | HCID 20583525 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 20583522 | HCID 20583522 | 39.1% |
Reaction Steps
A stirred of 665 mg (3.5 mmol) 4-chloro-thiazole-5-carboxylic acid ethyl ester, 416 mg (3.5 mmol) 3-cyanophenol, 2.4 g (7.3 mmol) Cs2CO3 and 60 mL dimethylformamide was warmed to 80° C. in an oil bath for 72 hours. The mixture was then cooled, poured into 70 mL water, and extracted with ethyl acetate (3×40 mL). The combined extracts were washed with water (2×50 mL), brine (1×50 mL), dried over Na2SO4, and concentrated via rotary evaporation. The resulting oil was chromatographed on a Biotage Flash 40S® silica column, loaded with methylene chloride and eluted with 20% ethyl acetate/80% hexanes to give 375 mg of a light yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06894041B2 |
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| Source dataset | uspto-grants-2005_05 |
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| ORD ID | ord-cf98d16ff9584e49aaa3c58b42f2fb3e |
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| Source note | uspto-grants-2005_05 |
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