HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl chloroformate → HCID 86745173, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 15096966 | HCID 15096966 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86745173 | HCID 86745173 | — |
Reaction Steps
A mixture of 3.0 parts of 5-[(4-fluorophenyl)methyl]-N-methyl-5H-imidazo[4,5-c]pyridin-2-amine, 2.4 parts of methyl carbonochloridate, 1.2 parts of N,N-diethylethanamine and 260 parts of dichloromethane was stirred for 2 days at room temperature. The reaction mixture was evaporated. The solid residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (94:6 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2-propanone, yielding 1 part of methyl [[5-[(4-fluorophenyl)methyl]-5H-imidazo[4,5-c]pyridin-2-yl]methyl]carbamate; mp. 178.8° C. (intermediate 98).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05137896 |
| Source dataset | uspto-grants-1992_08 |
| ORD ID | ord-a696cd70cd0045d7a3d6afec0067f690 |
| Source note | uspto-grants-1992_08 |