HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 46232721, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Trimethyl orthoformate | HCID 9005 | — |
| Reactant | HCID 25260758 | HCID 25260758 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 46232721 | HCID 46232721 | — |
Reaction Steps
To a solution of 1-methyl-3-{4-[4-(8-oxa-3-azabicyclo[3.2.1]oct-3-yl)-1-(4-oxocyclohexyl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]phenyl}urea (80 mg) (0.17 mmol) in DCM (2.0 mL) was added trimethylorthoformate and methanol in excess and a catalytic amount of p-toluene sulfonic acid along with molecular sieves and stirred at room temperature overnight. The added water and extracted 3 times with EtOAc. The organics were dried (MgSO4) and filtered off through a pad of Magnesol and concentrated in vacuo. to afford a solid. The solid was triturated with diethyl ether to give a white solid that was filtered and washed with diethyl ether to give (54 mg) MS m/z=476.2 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08129371B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-0574f33177414f839be0d3a47213a9af |
| Source note | uspto-grants-2012_03 |