HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylenediamine → 9-bromo-5H-pyrazino[2,3-b]indole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 1-Acetyl-4-bromoindolin-3-one | HCID 53243288 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 9-bromo-5H-pyrazino[2,3-b]indole | HCID 58880086 | 55.2% |
Reaction Steps
1-Acetyl-4-bromo-1,2-dihydro-indol-3-one (460 mg, 1.81 mmol) was dissolved in CH2Cl2 (8 mL). Bromine (111 μL, 2.2 mmol) was added slowly, and the reaction stirred for 20 min and then was concentrated in vacuo. The residue was dissolved in THF (8 mL). Ethylenediamine (244 μL, 3.6 mmol) was added, and the reaction stirred for 16 h at r.t. Triethylamine (2 mL) and MeOH (4 mL) were added, and the reaction stirred while left open to air for 24 h. The solution was concentrated in vacuo and purified by silica gel chromatography (8% MeOH/CH2Cl2) to give 248 mg (55%) of the title compound as a red solid. MS (ES) [m+H] calc'd for C10H6BrN3, 248, 250; found 248, 250.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08119655B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-494c14d48b4f44f4b9f1823f1a4c1869 |
| Source note | uspto-grants-2012_02 |