HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → HCID 57656859, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Benzyl piperazine-1-carboxylate | HCID 643495 | — |
| Reactant | HCID 57686771 | HCID 57686771 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 2-Methylpentane | HCID 7892 | — |
| Solvent | Butyronitrile | HCID 8008 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57656859 | HCID 57656859 | 70% |
Reaction Steps
tert-Butyl (2R)-2-{[(methylsulfonyl)oxy]methyl}morpholine-4-carboxylate (75 g, 0.25 mol), sodium iodide (11.4 g, 76 mmol), potassium carbonate (38 g, 0.28 mol) and benzyl-1-piperazine carboxylate (54 mL, 0.28 mol) were heated together in butyronitrile (1.5 L) at 115° C. for 24 hours. Water (1.8 L) was added and the layers separated, the aqueous phase was washed with ethyl acetate (1 L) and the combined organics were washed with brine (1 L), dried (MgSO4) and evaporated to give crude product as a yellow oil. Chromatography (5 kg column: 20% ethyl acetate to 50% ethyl acetate in isohexane) gave product as pale yellow gum (73 g, 0.17 mol, 70%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07906645B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-d2c65bf0605846d2b0c6e883a20333e0 |
| Source note | uspto-grants-2011_03 |