HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 58459083, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | HCID 67434553 | HCID 67434553 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58459083 | HCID 58459083 | 65.4% |
Reaction Steps
Add methyl chloroformate (0.29 g, 0.0031 mol) to a solution of 1-[8-(2-chlorophenyl)-2-methyl-6-piperazin-1-yl-purin-9-yl]-2-methyl-propan-2-ol (0.001 mol, 0.5 g) and pyridine (2.0 mL) in dry dichloromethane (3 mL) at 0° C. and stir for 2 h at room temperature. Quench the reaction mixture with saturated sodium bicarbonate solution and extract with dichloromethane. Dry the organic layer over anhydrous sodium sulfate, filter, and concentrate to give a residue. Purify the residue on a silica gel column using methanol:dichloromethane (3:97) as eluent to give Methyl 4-[8-(2-chlorophenyl)-9-(2-hydroxy-2-methyl-propyl)-2-methyl-purin-6-yl]piperazine-1-carboxylate (0.3 g). ES/MS m/z 459 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08759360B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-c6fad1490f714e42a3d668c55a1eca2d |
| Source note | uspto-grants-2014_06 |