HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 18706853, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | HCID 385223 | HCID 385223 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 18706853 | HCID 18706853 | 54.2% |
Reaction Steps
To 2-amino-6-chloro-4-[[(1-hydroxymethyl-1-cyclobutyl)methyl]amino]pyrimidine (0.24 g, 2.0 mmol) were added N-chlorosuccinimide (0.27 g, 2.0 mmol) and dimethylformamide (1.5 ml), and the mixture was stirred at room temperature for 2 days. Ethyl acetate was added and the mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=100:1) to give colorless prism crystals (0.3 g, 54.2%), m.p. 179-181° C. (acetone).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06080750 |
| Source dataset | uspto-grants-2000_06 |
| ORD ID | ord-225cb617e10e4cb4ba5b09eccd0edbd6 |
| Source note | uspto-grants-2000_06 |