HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 2753052, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | 1-Methylindene | HCID 13024 | — |
| Reactant | HCID 178418244 | HCID 178418244 | — |
| Catalyst | Titanium tetraisopropoxide | HCID 110612 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 2753052 | HCID 2753052 | — |
Reaction Steps
To a solution of 3.4 g of 1-methyl-1H-indene in 136 ml of ether was added 16.2 ml of a 1.62 M n-butyllithium/hexane solution at −78° C., followed by stirring at room temperature for 30 minutes. To the reaction mixture were added 15.5 ml of tetra-iso-propyl titanate and 2.41 ml of methyl chloroformate at −78° C., followed by stirring at −78° C. for 2 hours. To the reaction mixture were added 1 M hydrochloric acid and ethyl acetate to carry out a layer separation operation, followed by drying over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 1.57 g of methyl 1-methyl-1H-indene-1-carboxylate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447090B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-d4255b1769cd4469aad345cea7203b72 |
| Source note | uspto-grants-2016_09 |