HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178434607, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Bromo-5-(3-chloro-propyl)-3-methyl-pyrazole-1-sulfonic acid dimethylamide | HCID 66599631 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178434607 | HCID 178434607 | 91.1% |
Reaction Steps
To a solution of 4-bromo-5-(3-chloro-propyl)-3-methyl-pyrazole-1-sulfonic acid dimethylamide (3.85 g, 11.2 mmol) in MeOH (50 ml) at 0° C. was added 6 N HCl (50 mL). The reaction was warmed to room temperature and stirred overnight. The reaction was quenched by adding concentrated NH4OH until a pH of 8 was obtained. After concentrating to remove the MeOH, the remaining reaction solution was extracted with EtOAc and the organic layer was dried over Na2SO4, filtered and concentrated. The crude product was purified over normal phase silica starting with 10% EtOAc in heptane for 5 m and then increasing to 100% EtOAc over 40 m to give the desired product as a clear oil (2.42 g, 10.2 mmol). MS m/z 239.3 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598217B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-1bb0fc5b2d364c1688f48bae1f13d60a |
| Source note | uspto-grants-2013_12 |