HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 66690282, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 57433590 | HCID 57433590 | — |
| Reactant | HCID 66690761 | HCID 66690761 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66690282 | HCID 66690282 | 45.4% |
Reaction Steps
To a solution of methy 6-amino-4′-fluoro-5-nitrobiphenyl-3-carboxylate (0.42 g, 1.44 mmol) in N,N-dimethylformamide (4.8 mL) was added tin(1) chloride dihydrate (1.3 g, 5.8 mmol). The mixture was stirred at ambient temperature for 4 h and stored in the refrigerator for 18 h. Saturated ammonium chloride, water, and ethyl acetate were added. The mixture was extracted with ethyl acetate (3×). The combined organic layer was dried over magnesium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% dichloromethane→95% dichloromethane/methanol) gave the title compound (0.17 g): LC-MS [M+1]=261.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09238647B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-73ac188718724c1a94470788b466a658 |
| Source note | uspto-grants-2016_01 |