HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22932184, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3-Methyl-2-butanone | HCID 11251 | — |
| Reactant | Sodium amide | HCID 24533 | — |
| Reactant | (benzyloxy)(methylsulfanyl)methanethione | HCID 3415526 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 22932184 | HCID 22932184 | 71.7% |
Reaction Steps
A solution of S-methyl O-benzyl dithiocarbonate (6.90 g) and 3-methylbutan-2-one (3.00 g) in toluene (20 mL) was added dropwise to a suspension of sodium amide (2.71 g) in toluene (60 mL) at 0° C. over a 5-minute period. The mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into water, and the mixture was acidified by addition of 1 mol/L hydrochloric acid. The resulting mixture was extracted with diethyl ether, and the organic layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=10/1) to give the title compound (5.90 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07217697B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-946bf77e062e49c080fc546659a66dd5 |
| Source note | uspto-grants-2007_05 |