HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178512591, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Cyanamide | HCID 9864 | — |
| Reactant | 3-aMino-5-(trifluoroMethyl)phenol | HCID 14401229 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178512591 | HCID 178512591 | — |
Reaction Steps
A solution of 3-Amino-5-trifluoromethyl-phenol (0.21 g, 1.19 mmol), cyanamide (0.5 g, 1.19 mmol), 4N HCl in dioxane (2.975 ml, 1.199 mmol) in dioxane (10 ml) was heated in a sealed tube at 80° C. overnight resulting in complete conversion to product by TLC (10% MeOH:CH2Cl2). The reaction was partitioned between ethyl acetate/saturated NH4Cl solution and extracted. Some product remained in the aqueous phase after multiple extractions. The crude product (0.65 g, 0.297 mmol) was sufficiently pure by LC/MS to use directly for the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07276502B2 |
| Source dataset | uspto-grants-2007_10 |
| ORD ID | ord-50e4af14a0624ceb82c00a7cb7a22197 |
| Source note | uspto-grants-2007_10 |