HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 18187342, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 18187290 | HCID 18187290 | — |
| Solvent | Ethyl acetate hexane | HCID 21226206 | — |
| Product | HCID 18187342 | HCID 18187342 | 91.1% |
Reaction Steps
Method JJ: 2-Amino-N-(4-chlorophenyl)-3-(2,2-difluoropropionyl)pyridine (35) (190 mg, 0.640 mmol) was treated with conc. sulfuric acid (1 mL). The resulting red homogeneous solution was stirred at room temperature for 47.5 h. The reaction was quenched with saturated aqueous Na2CO3 (15 mL), and extracted with EtOAc (3×). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated in vacuo. Flash chromatography (50% EtOAc-hexane) provided 37 (173 mg, 91% yield) as an off-white solid (m.p. 188-190° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06593337B1 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-85f734a3de4c4f00adbd963d531a0db0 |
| Source note | uspto-grants-2003_07 |