HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl chloroformate → HCID 15654690, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Methyl 3-amino-2-(((2'-cyano-[1,1'-biphenyl]-4-yl)methyl)amino)benzoate | HCID 15654653 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 15654690 | HCID 15654690 | 90% |
Reaction Steps
To a stirred solution of methyl 3-amino-2-[(2′-cyanobiphenyl-4-yl)methylamino]benzoate (10 g) in pyridine (50 ml) was added dropwise methyl chloroformate (9.0 ml) under ice-cooling. The mixture was stirred at room temperature for 3 hours and concentrated. The residue was extracted with ethyl acetate. The extract was washed with water, dried and evaporated. The residue was recrystallized from ethyl acetate-hexane to afford pale yellow needles (10.5 g, 90%), m.p. 113-115° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06232334B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-9e6ed88f5da04fd4a1bcbf85084738fb |
| Source note | uspto-grants-2001_05 |