HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 9886858, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | HCID 86754985 | HCID 86754985 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 9886858 | HCID 9886858 | 56% |
Reaction Steps
A solution of 3.5 g of (±)-trans-N-[3-acetoxy-6-(4,4,4-trifluorobutoxy)-2,2-dimethylchroman-4-yl]-N-methyl-methanesulfonamide (example 21) and 6.8 g of DBU in 30 ml of toluene was heated at 105° C. for 20 h. The reaction mixture was diluted with EA and washed with hydrochloric acid until the aqueous phase gave an acidic reaction. The mixture was washed with sodium bicarbonate solution, dried over magnesium sulfate, concentrated i. vac. and triturated with heptane, giving 1.7 g N-[6-(4,4,4-trifluorobutoxy)-2,2-dimethyl-2H-chromen-4-yl]-N-methyl-methanesulfonamide; m.p. 118° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06008245 |
| Source dataset | uspto-grants-1999_12 |
| ORD ID | ord-994a84f893834e97b45ae9a0711edc0e |
| Source note | uspto-grants-1999_12 |