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 | US06355808B2 |
| Source dataset | uspto-grants-2002_03 |
| ORD ID | ord-3de6a647032f4e29b8bcc403f00701dd |
| Source note | uspto-grants-2002_03 |