HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19769440, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | HCID 19769443 | HCID 19769443 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19769440 | HCID 19769440 | 38.7% |
Reaction Steps
Potassium-t-butoxide (1.4 g) was added as a powder to an ice-cooled solution of N-[2,3,4,5-tetrahydro-1-(4-trifluoromethylphenoxy)-1H-3-benzazepin-3-yl]-trifluoroacet amide (4 g) in 100 mL tetrahydrofuran. After thirty minutes, dimethyl sulfate (1.5 g) was added. After warming to ambient temperature, the reaction mixture was stirred with water and extracted with ethyl acetate. The dried (anhydrous magnesium sulfate) organic layer was filtered and concentrated to 4.1 g solid, mp 210°-212°. A 2.5 g portion was recrystallized from acetonitrile to yield 1.6 g white crystals, mp 216°-218°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05202319 |
| Source dataset | uspto-grants-1993_04 |
| ORD ID | ord-0571d32facb141fbb3ce8c1b0deedf60 |
| Source note | uspto-grants-1993_04 |