HuagongsheHuagongshe Chemistry Print Report · For research reference only
Glyoxylic acid, monohydrate → HCID 73855624, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Glyoxylic acid, monohydrate | HCID 15620607 | — |
| Reactant | HCID 21949461 | HCID 21949461 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 73855624 | HCID 73855624 | 45.3% |
Reaction Steps
A slurry of 6-[4-methyl-2-(4-trifluoromethylphenyl)thiazol-5-ylmethylsulfanyl]-3,4-dihydro-2H-naphthalen-1-one (2.0 g, 4.6 mmol) in glyoxylic acid monohydrate (2.0 g, 22 mmol), under nitrogen atmosphere, was warmed to 160° C. and stirred for 1 h. The reaction mixture was cooled to room temperature, dissolved in EtOAc (100 mL) and filtered. The filtrate was washed with water (50 mL×3) and brine. The organic phase was dried over magnesium sulfate, concentrated under vacuum, and purified by recrystallization in ethanol to give 1.02 g (45%) of yellow solid. Analyzed for C24H18NO3S2: Calcd: C, 58.89%; H, 3.71%; N, 2.86%; Found: C, 58.715; H, 3.56%; N, 2.77.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07109222B2 |
| Source dataset | uspto-grants-2006_09 |
| ORD ID | ord-f1cfadb729034f85b6f889bde5cfedc1 |
| Source note | uspto-grants-2006_09 |