HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thioacetimidic acid 2-(4-methoxyphenyl)-2-oxoethyl ester hydrobromide → 4-(4-Methoxy-phenyl)-2-methyl-thiazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thioacetimidic acid 2-(4-methoxyphenyl)-2-oxoethyl ester hydrobromide | HCID 68489019 | — |
| Catalyst | Zincchloride | HCID 3007855 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | 4-(4-Methoxy-phenyl)-2-methyl-thiazole | HCID 768765 | 92.4% |
Reaction Steps
Heat a mixture of thioacetimidic acid 2-(4-methoxyphenyl)-2-oxoethyl ester hydrobromide (10.0 g, 32.9 mmol) and zinc (II) chloride (4.50 g, 33.0 mmol) in methanol (80 mL) at reflux under nitrogen protection for 6.5 hours. Cool the mixture, slowly dilute with saturated NaHCO3 (300 mL), and extract with methylene chloride (400 mL×2). Dry the combined organic extracts over sodium sulfate and remove the solvent under reduced pressure. Purify the crude product by flash column chromatography on silica gel, eluting with hexanes/ethyl acetate (9:1), to provide 4-(4-methoxyphenyl)-2-methylthiazole (6.24 g, 92%): APCI mass spectrum m/z 206 [C11H11NOS+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08552039B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-c7f894d5d3564aac93e3d5aee3c60438 |
| Source note | uspto-grants-2013_10 |