HuagongsheHuagongshe Chemistry Print Report · For research reference only
Butyl Chloride → HCID 14180639, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Butyl Chloride | HCID 8005 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | Carbamic acid, N-(4,6-dimethoxy-2-pyrimidinyl)-, phenyl ester | HCID 10945667 | — |
| Reactant | HCID 19863039 | HCID 19863039 | — |
| Catalyst | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14180639 | HCID 14180639 | 35.9% |
Reaction Steps
To 0.5 g of the product of Example 6, dissolved in 30 mL of p-doxane, was added 0.51 g of phenyl(4,6-dimethoxypyrimidin-2-yl)carbamate followed by 0.27 mL of "DBU". The reaction was stirred for 1.5 hours, diluted with 45 mL of ice-water and acidified with 10 drops of concentrated hydrochloric acid to obtain an oily precipitate. The water was decanted from the oil and the oily residue was dissolved in methylene chloride, washed with water and brine, and finally dried (MgSO4). Filtration and concentration of the filtrate, in vacuo, yielded an oil. Trituration with a 10:1 mixture of n-chlorbutane and methylene chloride provided 0.3 g of the subject compound as an off-white solid, m.p. 152°-54°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04759790 |
| Source dataset | uspto-grants-1988_07 |
| ORD ID | ord-bb257cdfd25c425e88b9d5e1b56bf1cc |
| Source note | uspto-grants-1988_07 |