HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 23372556, compound → HCID 22349637, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 23372556 | HCID 23372556 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 22349637 | HCID 22349637 | 72% |
Reaction Steps
To a solution of allyl 5-nitro-2-thiophenecarboxylate (3.2 g, 15 mmol) in concentrated hydrogen chloride (35 ml) were added under cooling SnCl2.H2O (10.1 g, 45 mmol). The mixture was stirred for 3.5 hours at ambient temperature, diluted with ethyl acetate and basified to pH 10 with 5N NaOH. The organic layer was washed with water and a saturated aqueous solution of sodium chloride, dried over MgSO4 and concentrated. The residue was purified by chromatography on silica gel using a mixture of ethyl acetate and petroleum ether (3:7) to give the title compound as a yellow oil (1.94 g, 72%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05527791 |
| Source dataset | uspto-grants-1996_06 |
| ORD ID | ord-30c2b7ed7e59453e8698289951bc8044 |
| Source note | uspto-grants-1996_06 |