HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57642823, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | HCID 11324599 | HCID 11324599 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57642823 | HCID 57642823 | 65.8% |
Reaction Steps
N-chlorosuccinimide (1.25 g) was added to a solution of 4-(9-methyl-9H-purin-6-yl)-piperazine-1-carboxylic acid t-butyl ester (2.70 g) in N,N-dimethylformamide (30 mL), and this was stirred at room temperature for 20 hours. Ethyl acetate (200 mL) and water (50 mL) were added, the organic layer was washed twice with 50 mL of water and then once with 50 mL of saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate. The organic layer was filtered and then concentrated under reduced pressure. The residue was purified by silica gel chromatography, and the ethyl acetate:hexane 4:1 fraction gave the title compound (1.97 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07524847B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-a95f75f465f8412d949b9309392e7548 |
| Source note | uspto-grants-2009_04 |