Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N,N~3~-Dimethyl-beta-alaninamide--hydrogen chloride (1/1) | HCID 25190939 | — |
| Reactant | HCID 54271004 | HCID 54271004 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 70629129 | HCID 70629129 | 155.2% |
Reaction Steps
A mixture of 16.1 g of 2-(methyl-chloroacetamido)-5-chlorobenzophenone, 10 g of triethylamine and 7.6 g of 3-methylaminopropionic acid methylamide hydrochloride in 500 ml of anhydrous xylene is heated to reflux for 12 hours whilst stirring. The triethylamine hydrochloride which has precipitated is filtered off with suction after cooling and, after extracting three times by shaking with water, the organic phase is dried over anhydrous potassium carbonate, filtered and evaporated in vacuo. The oily crude base thus obtained (18 g) is dissolved in 800 ml of anhydrous diethyl ether and filtered and 17.0 g of 2-(5-methylaminocarbonyl-N-methyl-3-methyl-3-aza-pentanamido)-5-chlorobenzophenone hydrochloride (77% of theory), with a melting point of 151°-153°, are obtained by passing dry hydrogen chloride into the solution.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04075409 |
|---|
| Source dataset | uspto-grants-1978_02 |
|---|
| ORD ID | ord-bd83244f89ce4795a04a52b00703d9cb |
|---|
| Source note | uspto-grants-1978_02 |
|---|