HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 21934672, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Amino-6-chloropyrimidine | HCID 238012 | — |
| Reactant | 1-(2-Methoxyethyl)piperazine | HCID 2734638 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 21934672 | HCID 21934672 | — |
Reaction Conditions
| Temperature | 125 °C |
|---|
Reaction Steps
6-Chloropyrimidin-4-amine 7-2 (0.3 g, 2.32 mmol) and diisopropylethylamine (0.30 g, 2.32 mmol) were suspended in n-butanol and then 1-(2-methoxyethyl)piperazine 5-2 (0.334 g, 2.32 mmol) was added. The reaction was stirred at 125° C. for 18 hours. The butanol was removed under reduced pressure, diluted with DCM and loaded onto a silica column eluted with DCM (100 mL), DCM:MeOH (99:4) and then DCM:MeOH:NH4OH (9:1:0.1). The product 5-3 was isolated after evaporation. 1H-NMR (DMSO): 7.95 ppm (s, 1H); 6.23 ppm (s, 2H); 5.59 ppm (s, 1H); 3.43 ppm (m, 4H); 3.33 ppm (m, 2H); 3.25 ppm (s, 3H); 2.59 ppm (m, 2H); 2.54 ppm (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115597B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-1e02db77e1c24b65ab44f24d9e983162 |
| Source note | uspto-grants-2006_10 |