HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 22914835, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 22914855 | HCID 22914855 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22914835 | HCID 22914835 | — |
Reaction Steps
A stream of gaseous methylamine is passed into a 250 ml round-bottomed flask containing a solution of 1.7 g (4.78 mmol) of methyl7-chloro-2-methyl-1-oxo-3-phenyl-1,2-dihydroisoquinoline-4-propanoate in 20 ml of dichloromethane and 80 ml of methanol until saturation and the mixture is left stirring at room temperature for 4 days. The solvents are evaporated under reduced pressure and the residue is purified by chromatography on a column of silica gel, elution being carried out with a mixture of dichloromethane and ethyl acetate ranging from 100/0 to 80/20 and then with a 95/5 mixture of dichloromethane and methanol. After recrystallizing from ethyl acetate, 1.36 g (3.83 mmol) of white solid are obtained. Melting point: 161°-162° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05665733 |
| Source dataset | uspto-grants-1997_09 |
| ORD ID | ord-a46bc0efdeb041fd9cf3917a0d390f64 |
| Source note | uspto-grants-1997_09 |