HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl dithiophosphate, potassium salt → HCID 71695284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl dithiophosphate, potassium salt | HCID 1385274 | — |
| Reactant | Methyl 3-cyano-4-methylbenzoate | HCID 11819538 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 71695284 | HCID 71695284 | 80.9% |
Reaction Steps
A solution of methyl 3-cyano-4-methylbenzoate (compound 1.7, 880 mg, 5.02 mmol, 1.00 equiv) and O,O′-diethyl dithiophosphate (1.41 g, 8.29 mmol, 1.50 equiv) in THF/H2O (40 mL) was stirred at 80° C. (CAUTION: significant gas evolution occurs—this and all other reactions described herein should be carried out in well ventilated fume hoods). After 3 h, the organic solvent was removed under reduced pressure and the residual aqueous phase was extracted with 3×20 mL of ethyl acetate. The combined organic layers were concentrated under reduced pressure to yield 0.85 g (79%) of the title compound as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08871790B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-dc3a1f2f247648e5844296f821f11e8f |
| Source note | uspto-grants-2014_10 |