HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 57855965, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 57855969 | HCID 57855969 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 57855965 | HCID 57855965 | — |
Reaction Steps
5-Methyl-6-nitro-2-trifluoromethyl-quinoline-7-carboxylic acid methyl ester (3.78 g, 12.03 mmol) are dissolved in 200 ml of methanol/water (3:1 mixture), and treated with lithium hydroxide hydrate (1.06 g, 0.046 mol) at room temperature. After reaction completion the mixture is poured into ethyl acetate and 2 N hydrochloric acid, the organic phase is washed three times with water, dried with sodium sulphate, filtered and concentrated in vacuo. The residue is triturated with a little hexane. Filtration gives 3.50 g (97% of theory) of the title compound as white crystals. 1H NMR (d6-DMSO3, 400 MHz): δ ppm: 2.65 (s, 3H); 8.25 (d, 1H); 8.56 (s, 1H); 9.05 ppm (d, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08580785B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-435abac5c4fe471abcfa9140db22385d |
| Source note | uspto-grants-2013_11 |