Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | HCID 19427680 | HCID 19427680 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 19427681 | HCID 19427681 | 42% |
Reaction Steps
To a solution of 11-cyclopropyl-4-methyl-6-trifluoromethanesulfonyloxy-11H-dipyrido[3,2-b:2',3'-e][1,4]diazepine (0.12 g, 0.3 mmol) in dioxan (1 mL) was added imidazole (0.06 g, 0.88 mmol). The mixture was heated at 100° C. for 10 min. After cooling to room temperature, the reaction mixture was diluted with ethyl adetate, washed with water, dried over sodium sulfate, filtered and concentrated. The residue was fractionated by preparative layer chromatography (silica gel, eluted with 67% ethyl acetate/hexane) to give the title compound (0.04 g, 0.12 mmol, 42%) which crystallized from di-isopropyl ether, m.p. 198°-200° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05550117 |
|---|
| Source dataset | uspto-grants-1996_08 |
|---|
| ORD ID | ord-3b16c01633f34d35aa0a5c6692c1f568 |
|---|
| Source note | uspto-grants-1996_08 |
|---|