HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-Bromo-5-(p-chlorophenyl)-4-nitro-2-[(trifluoromethyl)thio]pyrrole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 2-(p-Chlorophenyl)-3-nitro-5[(trifluoromethyl)thio]pyrrole | HCID 18930387 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 3-Bromo-5-(p-chlorophenyl)-4-nitro-2-[(trifluoromethyl)thio]pyrrole | HCID 18930447 | 56.6% |
Reaction Steps
A solution of 2-(p-chlorophenyl)-3-nitro-5-[(trifluoromethyl)thio]pyrrole (0.35 g, 0.0011 mol) and sodium acetate (0.11 g, 0.0013 mol) in acetic acid is treated with a solution of bromine (0.21 g, 0.0013 mol) in acetic acid, stirred for one hour, poured into water and extracted with ethyl acetate. The combined organic extracts are washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a residue. Flash chromatography of the residue using silica gel and a 1:9 ethyl acetate/hexanes solution gives the title product as a yellow solid (0.25 g, mp 160°-165° C.) which is identified by 1HNMR, 19FNMR 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-09530907c1c648b6975fcafa7758157c |
| Source note | uspto-grants-1996_01 |