HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Cyanophenol → HCID 11805868, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Cyanophenol | HCID 13019 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Dimethylthiocarbamoyl chloride | HCID 27871 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 11805868 | HCID 11805868 | 75% |
Reaction Steps
Add sodium hydride (1.21 g, 95%) to a solution of 4-cyanophenol (5.71 g, 47.98 mmol) in anhydrous TI-IF (70 mL) and stir the mixture for 5 min. Add dimethylthiocarbamoyl chloride (5.93 g, 47.98 mmol) and heat the mixture at reflux for 3 h. Cool the mixture to room temperature and add water. Extract the aqueous phase with EtOAc, dry the organic phase over MgSO4, filter and concentrate in vacuo to obtain a solid. Wash the solid with diethyl ether, filter and dry in vacuo to obtain the desired intermediate as a solid (4.41 g, 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680091B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-4c0a99a32c55495fbf1fd57316a7fcaf |
| Source note | uspto-grants-2014_03 |