Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 10672079 | HCID 10672079 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 11797134 | HCID 11797134 | 101.5% |
Reaction Steps
130 mg (0.276 mmol) of Compound 160 obtained in EXAMPLE 160 was dissolved in 5 mL of dimethylformamide, 112 mg (1.38 mmol) of dimethylamine hydrochloride and 0.24 mL (1.38 mmol) of diisopropylethylamine were added, and the mixture was stirred at 50° C. for 30 minutes. Water was added to the reaction solution and the mixture was extracted with ethyl acetate. The organic layer was washed with water and an aqueous saturated solution of sodium chloride and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=9:1), to give 122 mg of Compound 162 (yield: 86%), which was converted to a hydrochloride according to the same manner as that in EXAMPLE 161.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05539112 |
|---|
| Source dataset | uspto-grants-1996_07 |
|---|
| ORD ID | ord-76ec97d07a964a3991fda263204ddeb5 |
|---|
| Source note | uspto-grants-1996_07 |
|---|