HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 70664923, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Ethyl 5-amino-1-phenyl-1H-pyrazole-3-carboxylate | HCID 23630921 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 70664923 | HCID 70664923 | — |
Reaction Steps
500 mg (2.0 mmol) of 5-Amino-1-phenyl-1H-pyrazole-3-carboxylic acid ethyl ester are dissolved in 10 ml of THF, 0.56 ml (4.0 mmol) of triethylamine and 230 mg (2.0 mmol) of methanesulfonyl chloride are added. The mixture is stirred overnight at RT, the solvent is removed in vacuo and the crude product is subjected to an aqueous work-up and extracted with dichloromethane. The isolated product is dissolved in 10 ml of DMF, 8 mmol 12.5 mmol of 1M NaOH solution are added and the mixture is stirred overnight at RT. The solvent is removed in vacuo and the crude product subjected to HPLC chromatography. Yield after two steps: 170 mg, 30%
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08962671B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-e07c8a1fd36e4e84a14e6f5366ac21e9 |
| Source note | uspto-grants-2015_02 |