HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Acetamide, 2-(diphenylphosphinothioyl)-N,N-diethyl-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Chloro-N,N-diethylacetamide | HCID 16844 | — |
| Reactant | HCID 178528040 | HCID 178528040 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Acetamide, 2-(diphenylphosphinothioyl)-N,N-diethyl- | HCID 796778 | — |
Reaction Steps
A stirred mixture of diphenylphosphine sulfide (4.365 g, 0.02 mol) and N,N-diethylchloroacetamide (4.189 g, 0.028 mol) in methylene chloride (80 ml) was cooled to 8–10° C. in an ice-water bath. Small pieces of solid potassium hydroxide (3.927 g, 0.07 mol) were added while stirring under nitrogen atmosphere. After 30 minutes, water (25 ml) was added and the organic layer was separated, washed with more water (25 ml) and dried over sodium sulfate. The solvent was removed under reduced pressure using a rotary evaporator and the oily residue was crystallized from ethyl acetate-hexane mixture to give 3.5 g (53%) of large cubes. mp: 108–110° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07157219B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-415fe52e9f254e298e86d93ccb87466a |
| Source note | uspto-grants-2007_01 |