HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 24904076, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 53742305 | HCID 53742305 | — |
| Solvent | Ethyl orthoformate | HCID 31214 | — |
| Product | HCID 24904076 | HCID 24904076 | — |
Reaction Steps
6.5 g (25.7 mmol) of 5-amino-2-chloro-4-[N-(2-fluorobenzyl)-amino]-pyrimidine are dissolved at room temperature in 65 ml of triethyl orthoformate. 30 mg of methanesulfonic acid are added to the solution and the reaction mixture is then stirred for 15 hours at room temperature. The reaction mixture is then concentrated by evaporation and the residue is chromatographed on silica gel with toluene/ethyl acetate (3:1) as eluant. The eluate is concentrated by evaporation and the residue obtained is recrystallised from dichloromethane/diethyl ether. In this manner 2-chloro-9-(2-fluorobenzyl)-9H-purine is obtained in the form of colourless crystals having a melting range of from 103° to 104°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05110818 |
| Source dataset | uspto-grants-1992_05 |
| ORD ID | ord-62115ab0c7504e6ebd113538db6f267a |
| Source note | uspto-grants-1992_05 |