HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 54204871, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | Sodium methanethiolate | HCID 4378561 | — |
| Reactant | HCID 54388633 | HCID 54388633 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 54204871 | HCID 54204871 | 50.1% |
Reaction Steps
Sodium thiomethoxide (6.83 g) was added to a solution of methyl 2-fluoro-3-methoxycarbonyl-4-trifluoromethylbenzoate (24.85 g) in xylene. After stirring for 0.5 hours lithium hydroxide monohydrate (4.10 g) was added and the mixture was stirred for 48 hours. Hydrochloric acid (2M) was added. It was extracted with ether, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was triturated with cyclohexane. The solid was filtered off and the filtrate was evaporated to dryness to give methyl 3-methoxycarbonyl-2-(methylsulphenyl)-4-trifluoromethylbenzoate (13.71 g) as a yellow oil NMR (CDCl3) 2.4(s,3H), 3.95 (s,6H), 7.65 (s,2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05650533 |
| Source dataset | uspto-grants-1997_07 |
| ORD ID | ord-03697e6ae9f0465b99c4012ae101e632 |
| Source note | uspto-grants-1997_07 |