HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 53971866, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 54084237 | HCID 54084237 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 53971866 | HCID 53971866 | — |
Reaction Steps
A mixture of 4-(N-butylcarbamoyl)methylidene-4,5,6,7-tetrahydrobenzo[b]thiophene-2-carboxylic acid (0.57 g), conc. sulfuric acid (H2SO4) (3 ml), and methanol (MeOH) (15 ml) was stirred at reflux for 1.5 hours. The reaction mixture was poured into a mixture of AcOEt and water. The organic layer was washed with saturated aqueous solution of NaHCO3, water and brine, and dried over MgSO4, and evaporated in vacuo. After evaporation, the resulting oil was purified by chromatography on silica gel (AcOEt-n-hexane as an eluent). The fractions including the object compound were collected and evaporated to give 4-(N-butylcarbamoyl)methylidene-2-methoxycarbonyl-4,5,6,7-tetrahydrobenzo[b]thiophene (115.3 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06274619B1 |
| Source dataset | uspto-grants-2001_08 |
| ORD ID | ord-85c385d4219a4177886d2a8e26e0d975 |
| Source note | uspto-grants-2001_08 |