HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 73214617, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-Methyl-2,7-diazaspiro(4.4)nonane | HCID 4713500 | — |
| Reactant | Avanafil Impurity K | HCID 86342163 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 73214617 | HCID 73214617 | 4% |
Reaction Steps
In DCM (30 mL) were dissolved 4-((3-chloro-4-methoxybenzyl)amino)-2-(methylsulfinyl)-N-(pyrimidin-2-ylmethyl)pyrimidine-5-formamide (429 mg, 0.96 mmol) and DIEA (0.22 mL, 1.12 mmol). 2-Methyl-2,7-diazaspiro[4.4]nonane (154 mg, 1.1 mmol) was then added. The reaction was conducted at ambient temperature overnight. The solvent was removed by rotary evaporation, followed by addition of water and extraction with ethyl acetate. The organic phase was dried over sodium sulfate and purified by silica gel column chromatography (DCM/methanol=20/1 to 10/1) to give a white solid (20 mg, 4% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09359371B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-c60a9ccf37364aeaa81803ca0a5500f8 |
| Source note | uspto-grants-2016_06 |