HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium thiocyanate → HCID 18930395, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium thiocyanate | HCID 15666 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 378974 | HCID 378974 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 18930395 | HCID 18930395 | 84.9% |
Reaction Steps
A solution of ethyl 5-(p-chlorophenyl)pyrrole-2-carboxylate (0.95 g, 3.8 mmol) in acetic acid (20 mL) is treated with ammonium thiocyanate (1.75 g, 22.8 mmol), stirred at room temperature for five minutes, cooled to 15° C., treated with a solution of bromine (0.91 g, 5.7 mmol) in acetic acid (10 mL) and stirred at room temperature for several hours. The reaction mixture is filtered to remove solids and the filtrate is poured into water and stirred. The aqueous mixture is filtered to obtain an off-white solid. Flash chromatography of the solid using a 1:10 ethyl acetate/hexanes solution gives the title product as a white solid (0.99 g, mp 138°-141° C.) which is identified by 1HNMR and 13CNMR spectral analyses.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05484807 |
| Source dataset | uspto-grants-1996_01 |
| ORD ID | ord-d6d6ba4a09cf4897af41f930af45ca0a |
| Source note | uspto-grants-1996_01 |