HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68934618, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | HCID 57531656 | HCID 57531656 | — |
| Solvent | Ethyl formate | HCID 8025 | — |
| Product | HCID 68934618 | HCID 68934618 | 79.1% |
Reaction Steps
A solution of ethyl 1,5,5-trimethyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate (1.00 g, 4 mmol) in anhydrous ethyl formate (10 mL) was treated with sodium ethoxide (0.54 g, 8 mmol) and refluxed for 3 hours. The mixture was cooled to room temperature and poured into cold water (40 mL). The aqueous layer was washed with diethyl ether (40 mL) to remove unreacted starting material, acidified with a 20% NaH2PO4 solution and extracted with ethyl acetate (50 mL×2). The organic extracts were collected, dried on Na2SO4 and evaporated to dryness to obtain the title compound (0.88 g, 78.8% yield) as a brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08541429B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-6dcce04b4e824615b3a58ff6811cf1f2 |
| Source note | uspto-grants-2013_09 |