HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-(Trifluoromethoxy)benzenemethanol → HCID 69141711, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-(Trifluoromethoxy)benzenemethanol | HCID 137184 | — |
| Reactant | 2-((1,1-Dimethylethyl)imino)-N,N-diethylhexahydro-1,3-dimethyl-2lambda5-1,3,2-diazaphosphorin-2-amine | HCID 3513851 | — |
| Reactant | Tert-butyl 4-(chlorocarbonyl)piperazine-1-carboxylate | HCID 11334154 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 69141711 | HCID 69141711 | — |
Reaction Steps
652 mg (1.5 mmol) PS-BEMP and 373 mg (1.5 mmol) 4-chlorocarbonyl-piperazine-1-carboxylic acid tert-butyl ester was added to a solution of 192 mg (1.0 mmol) 4-trifluoromethoxybenzyl alcohol in 5 ml acetonitrile. The mixture was heated to reflux for 24 h then cooled to rt, diluted with 5 ml acetonitrile, 666 mg (4.5 mmol) PS-NH2 added and shaken at rt for 16 h. After filtration and evaporation the crude product is purified by flash chromatography on silica gel with hexane/AcOEt 50:50: 180 mg colourless crystalline solid. 1H-NMR (CDCl3): 1.45 s, 9H, 3.35–3.55 m, 8H, 5.14 s, 2H, 7.20 d, 2H and 7.40 d, 2H, AB-system.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07022707B2 |
| Source dataset | uspto-grants-2006_04 |
| ORD ID | ord-e99f606e8e264e1a87617001d9106f85 |
| Source note | uspto-grants-2006_04 |