HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Aminothiophenol → HCID 9882434, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Aminothiophenol | HCID 8713 | — |
| Reactant | methyl 2-methyl-4,6-dioxocyclohexanecarboxylate | HCID 4661376 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 9882434 | HCID 9882434 | — |
Reaction Steps
A mixture of methyl 6-methyl-2,4-dioxocyclohexane-1-carboxylate, 7a (5.52 g, 30 mmole) and 2-aminothiophenol, 6 (X=H, 3.75 g, 30 mmole), in DMSO (10 mL) is placed in a preheated heating mantle. The reaction mixture is stirred and refluxed for 0.5 h. Upon cooling, the reaction mixture forms a solid. The crystals are filtered and the remaining mother liquid is poured into cold water, whereupon further precipitation occurs. Each precipitate is separately recrystallized twice from MeOH and proves to be identical. An analytical sample of 4a, (R=H), mp 218-221° C. occurs as light orange crystals; yield: 1.47 g (55.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05994349 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-79527183e05f4a8ebd53f39c1964f295 |
| Source note | uspto-grants-1999_11 |