HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosulfonic acid → HCID 89826088, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosulfonic acid | HCID 24638 | — |
| Reactant | 3-(2-Bromo-3,5-difluorophenyl)propanoic acid | HCID 84045984 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 89826088 | HCID 89826088 | 96.6% |
Reaction Steps
3-(2-Bromo-3,5-difluorophenyl)propanoic acid (from Step 2, 3.0 g) is stirred with chlorosulfonic acid (10 mL) for 2 hours at ambient temperature. The mixture is then added dropwise to a vigorously stirred mixture of water and ice (200 mL) and further stirred for 15 minutes. Extraction with diethyl ether, subsequent washing of the organic layer with water, NaOH (0.2 M), and brine, drying (Na2SO4) and removal of the solvent under reduced pressure gives the crude product (Yield 2.7 g) that is used in the next step without further purification. LC (METHOD 7): tR=1.16 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09308194B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-38fefd198f4e4375b47069535a6c9d60 |
| Source note | uspto-grants-2016_04 |