HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine, hydrochloride → HCID 11432721, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | Methyl 4-(acetylamino)-6(4-chlorophenyl)-7-(2,4-dichlorophenyl)-1-methyl-2-oxo-1,2-dihydro-1,8-naphthyridine-3-carboxylate | HCID 11307094 | — |
| Reactant | Trimethylaluminum | HCID 16682925 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 11432721 | HCID 11432721 | — |
Reaction Steps
To dimethylamine hydrochloride (26.1 mg) in toluene (2 mL) was added Al(CH3)3 (0.16 mL) at 0° C. The reaction stirred for about 30 minutes before adding the product of EXAMPLE 91 (85 mg) in toluene (1 mL). The reaction stirred for 3.5 hours at 50° C. and was quenched with aqueous 1 M HCl. The reaction was diluted with EtOAc washed with aqueous 1 M HCl. The solution was dried (Na2SO4) and concentrated. The concentrated residue was purified by preparative TLC on silica gel eluted with 6% methanol in CH2Cl2 affording the title compound. HPLC/MS: 543.0 (M+1), 545.0 (M+3); Rt=3.51 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07728141B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-c28aed103c1d4bb9b51add5a63dc8396 |
| Source note | uspto-grants-2010_06 |