HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 22404729, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ethyl 3-amino-4,4,4-trifluorocrotonate | HCID 5702529 | — |
| Reactant | HCID 22404735 | HCID 22404735 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22404729 | HCID 22404729 | 36.9% |
Reaction Steps
By the method of Example 1, Step G, 4.0 grams (0.016 mole) of 5-chloro-3,4-dihydro-2,2-dimethyl-7-fluoro-2H-1-benzopyran-8-yl isocyanate was reacted with 1.0 gram (0.023 mole) of sodium hydride and 3.0 grams (0.017 mole) of ethyl 3-amino-4,4,4-trifluorocrotonate in 150 mL of tetrahydrofuran. Subsequently, 4.5 grams (0.032 mole) of methyl iodide and 4.4 grams (0.032 mole) of potassium carbonate were reacted with the product of the first reaction, yielding 2.4 grams of 3-(5-chloro-3,4-dihydro-2,2-dimethyl- 7-fluoro-2H-1-benzopyran-8-yl)-1-methyl-6-trifluoromethyluracil, mp 132°-135° C. The NMR spectrum was consistent with the proposed structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05521147 |
| Source dataset | uspto-grants-1996_05 |
| ORD ID | ord-212e55230c9f413b9070cee89436b8f2 |
| Source note | uspto-grants-1996_05 |