HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 68108477, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | Methyl 3-cyano-5-cyclopropyl-4-methoxybenzoate | HCID 68108310 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68108477 | HCID 68108477 | 85.4% |
Reaction Steps
Methyl 3-cyano-5-cyclopropyl-4-methoxybenzoate (491 mg) was dissolved in tetrahydrofuran (7.5 mL) and water (2.5 mL), and lithium hydroxide monohydrate (359 mg) was added to the solution, and then the mixture was stirred at mom temperature for 20 hours. The organic solvent was distilled off under reduced pressure and the aqueous layer was washed with n-hexane. To the aqueous layer, 1N hydrochloric acid was added, and the mixture was extracted with ethyl acetate under acidic conditions. The organic layer was washed with saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (394 mg) as a pale brown crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367843B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-d3217d6cc8fb41e2aacd9263d1409a95 |
| Source note | uspto-grants-2013_02 |