HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 13885368, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Methyl (4,6-dimethoxy-1,3,5-triazin-2-yl)carbamate | HCID 12803256 | — |
| Reactant | HCID 13885367 | HCID 13885367 | — |
| Reactant | Trimethylaluminum | HCID 16682925 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 13885368 | HCID 13885368 | 23.8% |
Reaction Steps
In a dry flask under nitrogen was placed 1.20 gram of 2-(azetidin-1-ylsulfonyl)benzenesulfonamide, 50 ml of dry dichloromethane and 2.48 ml of 2M trimethylaluminum in toluene. To this was added 0.885 g of 4,6-dimethoxy-1,3,5-triazin-2-ylcarbamic acid methyl ester and the resultant solution was heated to reflux for 12 hours. The solution was washed with 50 ml of a water/acetic acid/1N HCl solution (40:10:0.4). The organic fraction was concentrated and chromatographed on silica gel (ethyl acetate/methylene chloride (15:85)). The slower moving portions were collected, treated with ethyl acetate and dried to give 0.45 g of a solid, m.p. 175°-177° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04786316 |
| Source dataset | uspto-grants-1988_11 |
| ORD ID | ord-92147a67b1644334a1b9b71153d57211 |
| Source note | uspto-grants-1988_11 |