HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → HCID 58790234, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | 4-Bromo-N-(2-chloroethyl)-N-methylbenzenemethanamine | HCID 58790392 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 58790234 | HCID 58790234 | 69.1% |
Reaction Steps
To a solution of 73 (3.5 g, 13.3 mmol) in DME (20 ml) was added N-methylpiperazine (3.33 g, 2.5 eq, 33.3 mmol) and tetrabutylammonium bromide (cat). The reaction mixture was heated to reflux for 3 hrs, then cooled to RT and concentrated. The crude was dissolved in EtOAc, washed well with water and the organic phase was collected, dried over Na2SO4 and filtered then concentrated. Purification by column chromatography (20% MeOH in EtOAc+1% TEA) afforded 74 as colorless oil (3.0 g, 69% yield). MS (m/z): 326.0/328.0 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08093264B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-cc47b3174e814604b746ecf7f09820ae |
| Source note | uspto-grants-2012_01 |