HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 67201273, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3,5-Difluorobenzenesulfonyl chloride | HCID 2774058 | — |
| Reactant | HCID 67202227 | HCID 67202227 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67201273 | HCID 67201273 | 92.1% |
Reaction Steps
To a suspension of 3-amino-4,5,6,7-tetrahydro-pyrazolo[4,3-c]pyridine-2-carboxylic acid ethyl ester hydrochloride (36.2 g, 127.8 mmol) in anhydrous dichloromethane (1 L), at 0°-5° C., N,N-diisopropylethylamine (111.3 mL, 639 mmol) was added. To the resulting solution, 3,5-difluorobenzenesulfonyl chloride (27.17 g, 127.8 mmol) was added portionwise. The mixture was stirred at 0°-5° C. for 1 hour then at room temperature for 3 hours. The organic phase was washed with NaHCO3 saturated solution, water and brine, dried over sodium sulfate filtered and evaporated. The crude, was triturated with diethylether (500 mL) to obtain the title compound as yellowish solid (45.48 g, 92%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07947686B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-63dc50912c84462c97fade7b4e80aadd |
| Source note | uspto-grants-2011_05 |