HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → [4-(Methanesulfonylaminocarbonyl)butyl]triphenylphosphonium bromide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 5-Bromo-N-methanesulfonylpentanamide | HCID 20296141 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | [4-(Methanesulfonylaminocarbonyl)butyl]triphenylphosphonium bromide | HCID 19608840 | 63.7% |
Reaction Steps
A solution of 2.20 g. (8.57 mmoles) of the N-methanesulfonyl-5-bromovaleramide, prepared as above, 2.24 g. (8.57 mmoles) of triphenylphosphine, and 20 ml. of acetonitrile was heated to reflux under nitrogen overnight. The solution was then concentrated by rotary evaporation and the resultant solid was triturated with hot benzene (4×). The triturated solid was recrystallized from absolute ethanol:ether to afford the white, crystalline [4-(methanesulfonylaminocarbonyl)butyl]triphenylphosphonium bromide weighing 2.80 g. (63.7% yield) melting at 190°-191°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04244887 |
| Source dataset | uspto-grants-1981_01 |
| ORD ID | ord-403257624a504678b4c14a3beb204b41 |
| Source note | uspto-grants-1981_01 |