HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 21812870, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 21812866 | HCID 21812866 | — |
| Reactant | HCID 131731131 | HCID 131731131 | — |
| Catalyst | Tetrabutylammonium Chloride | HCID 70681 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21812870 | HCID 21812870 | 23% |
Reaction Steps
(Z)-3-amino-4,4-dimethyl-pent-2-enenitrile (26 g, 209.35 mmol), sodium sulfide decahydrate (5.71 g, 73.27 mmol) and tetrabutyl ammonium chloride (9.31 g, 33.49 mmol) in benzene and water (215 mL, 2.5:1, v/v) is stirred at 75° C. under hydrogen sulfide gas for three days. 200 mL of ethyl acetate is added and the layers separated. The organic layer is washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure to afford the title compound. Yield 23% over three steps. ESI m/z 159=MH+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629157B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-3730f2159afd4d9ebc6d4a3b7243e6e7 |
| Source note | uspto-grants-2014_01 |