HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 33779600, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | Methyl 3-chloro-5-cyano-4-methoxybenzoate | HCID 68108614 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 33779600 | HCID 33779600 | 98.9% |
Reaction Steps
Methyl 3-chloro-5-cyano-4-methoxybenzoate (1.02 g) was dissolved in tetrahydrofuran (15 mL) and water (6 mL), and lithium hydroxide monohydrate (759 mg) was added to the solution, and then the mixture was stirred at room temperature for 90 minutes. The organic solvent was distilled off and the aqueous layer was washed with n-hexane. The aqueous layer was acidified with 1N hydrochloric acid and then extracted with ethyl acetate. 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 (946 mg) as a colorless crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367843B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-3eaa206d58df4fa5af41816689591f14 |
| Source note | uspto-grants-2013_02 |