Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl isocyanatoacetate | HCID 76283 | — |
| Reactant | HCID 178516560 | HCID 178516560 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178472768 | HCID 178472768 | — |
Reaction Steps
5-Fluoro-4-hydroxy-thiochromen-2-one (500 mg, 2.55 mmol) was placed in a CEM Microwave vessel and suspended in anhydrous DCM (5 mL.) Triethylamine (710 uL, 5.1 mmol) and isocyanato-acetic acid ethyl ester (572 uL, 5.1 mmol) were added in one portion and the reaction heated to 120° C. in a CEM Discovery Microwave system. After three hours, the reaction was cooled diluted with 10 volumes of dichloromethane, washed with an equal volume of 1N HCl and dried over magnesium sulfate to provide the title compound which was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09149476B2 |
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| Source dataset | uspto-grants-2015_10 |
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| ORD ID | ord-08a01cc0ff114b21b3359ee4aac802b1 |
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| Source note | uspto-grants-2015_10 |
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