HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tin tetrachloride → HCID 178470016, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tin tetrachloride | HCID 24287 | — |
| Reactant | Triethyl methanetricarboxylate | HCID 80471 | — |
| Reactant | 3-Methoxybenzenethiol | HCID 84989 | — |
| Solvent | Dichloromethane ethylacetate | HCID 21226138 | — |
| Product | HCID 178470016 | HCID 178470016 | 5.5% |
Reaction Conditions
| Temperature | 210 °C |
|---|
Reaction Steps
SnCl4 was added to a neat mixture of 3-methoxy-benzenethiol (0.91 g, 6.5 mmol) and 2-ethoxycarbonyl-malonic acid diethyl ester (2.27 g, 9.77 mmol) in a 20-mL open vial. The reaction mixture was heated in a 210° C. oil bath for 2.5 h. After cooling, the reaction mixture was subjected to silica gel chromatography (3%-50% EtOAc/CH2Cl2) to provide 4-hydroxy-7-methoxy-2-oxo-2H-thiochromene-3-carboxylic acid ethyl ester (100 mg). MS ESI(+) m/e: 281.10 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08927591B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-614112b392c941fa8feacc384c848817 |
| Source note | uspto-grants-2015_01 |