HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 19427668, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 19427680 | HCID 19427680 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 19427668 | HCID 19427668 | 30% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
To a solution of 11-cyclopropyl-4-methyl-6-trifluoromethanesulfonyloxy-11H-dipyrido[3,2-b:2',3'-e][1,4]diazepine (0.22 g, 0.55 mmol) in 1,4-dioxane (3 mL) was added 30% ammonium hydroxide (3 mL). The mixture was heated at 100° C. for 15 min. After cooling to room temperature the mixture was diluted with ethyl acetate, washed with water, dried (magnesium sulfate), filtered and concentrated in vacuo. The residue was chromatographed over silica gel (eluted with 1:1:1 ethyl acetate/hexane/methylene chloride→50% ethyl acetate/hexane) to give the title compound (0.045 g, 0.17 mmol, 30%) which crystallized from ethyl acetate/hexane, m.p. 242°-244° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05550117 |
| Source dataset | uspto-grants-1996_08 |
| ORD ID | ord-09ceb7c8182a42de9faab1031432f103 |
| Source note | uspto-grants-1996_08 |