HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → 3-(Methylcarbamoyl)isoxazol-5-ylmethyl 2-(6-fluoroquinolin-2-yl)-2-azaspiro[3.3]hept-6-ylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Ethyl 5-[2-(6-Fluoroquinolin-2-yl)-2-azaspiro[3.3]hept-6-ylcarbamoyloxymethyl]isoxazole-3-carboxylate | HCID 68000144 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 3-(Methylcarbamoyl)isoxazol-5-ylmethyl 2-(6-fluoroquinolin-2-yl)-2-azaspiro[3.3]hept-6-ylcarbamate | HCID 46850978 | — |
Reaction Steps
In a sealed tube, a solution of 0.130 g (0.28 mmol) of ethyl 5-[2-(6-fluoroquinolin-2-yl)-2-azaspiro[3.3]hept-6-ylcarbamoyloxymethyl]isoxazole-3-carboxylate, prepared in step 11.9., in 4.13 mL (28.01 mmol) of a solution (8M) of methylamine in ethanol, is stirred at room temperature for 5 hours. The mixture is evaporated to dryness. The residue obtained is crystallized from hot ether. The precipitate thus formed is filtered off and rinsed thoroughly with ether. After drying under vacuum at about 60° C., 0.05 g of pure product is obtained in the form of a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08889702B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-d09addc233e64d72b63854c2ec3ac812 |
| Source note | uspto-grants-2014_11 |