HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 13279244, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 13279243 | HCID 13279243 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 13279244 | HCID 13279244 | — |
Reaction Steps
8.0 g of N-propargyl-N-(4,6-dimethyl-2-dimethylamino-pyrimidin-5-yl)-hydroxyacetamide, 3.7 g 4-dimethylaminopyridine and 100 ml dry CH2Cl2 are charged in a sulphonation flask. Thereto are added, dropwise, 3.43 g mesyl chloride in 30 ml of dry CH2Cl2. The reaction temperature rises from 22° up to 33°. The mixture is heated under reflux for 34 hours, cooled and diluted with water. The organic phase is partitioned off, dried over Na2SO4 and evaporated. The oily residue is chromatographed on silica gel with diethylether/hexane 1:1 to give the title compound, m.p. 108°-110°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04657579 |
| Source dataset | uspto-grants-1987_04 |
| ORD ID | ord-166bcbc52c784528add8f0d3e14151ad |
| Source note | uspto-grants-1987_04 |