Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | 2-Fluoro-4-iodoaniline | HCID 185694 | — |
| Reactant | 1-Methylhomopiperazine | HCID 228349 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Solvent | Dichloromethane methanol ammonium hydroxide | HCID 21896990 | — |
| Product | HCID 69052994 | HCID 69052994 | — |
Reaction Steps
A mixture of 2-fluoro-4-iodoaniline (474 mg, 2.00 mmol), 1-methylhomopiperazine (0.372 mL, 3.00 mmol), ethylene glycol (0.222 mL, 4.00 mmol) and K3PO4 (848 mg, 4.00 mmol) in isopropanol (2 mL) was degassed with Ar before being charged with CuI (76 mg, 0.40 mmol). The mixture in a sealed tube was heated at 85° C. for three days. One fifth of the reaction mixture was applied to a silica gel prep TLC plate, which was then developed in CH2Cl2/MeOH/NH4OH (85/15/0.5). The area containing the desired product was scraped out, and the product was extracted out with CH2Cl2/MeOH (2/1) to give a solid (54 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07612089B2 |
|---|
| Source dataset | uspto-grants-2009_11 |
|---|
| ORD ID | ord-79222ea8596d4c4ba7fec1b3607097dc |
|---|
| Source note | uspto-grants-2009_11 |
|---|
