HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 57703895, compound → HCID 24751332, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 57703895 | HCID 57703895 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Boron tribromide | HCID 25134 | — |
| Product | HCID 24751332 | HCID 24751332 | 67.5% |
Reaction Steps
A solution of 5-(3-fluoro-benzenesulfonyl)-3-[3-[(2-methoxy-ethyl)-methyl-amino]-4-(4-methyl-piperazin-1-yl)-benzoylamino]-5,6-dihydro-4H-pyrrolo[3,4-c]pyrazole-1-carboxylic acid ethyl ester (120 mg, 0.186 mmol) in 5 mL of 1M BBr3 in dichloromethane was stirred at room temperature for 24 h. The mixture was washed with saturated aqueous NaHCO3 and the combined organic layers were evaporated to dryness. The resulting crude (110 mg) was then dissolved in 4 mL of MeOH and 0.5 mL of triethylamine and the mixture was stirred at room temperature for 3 h. The solvent was removed and the final product was purified by flash column chromatography, using dichloromethane-methanol-aqueous ammonia 9:1:0.5 as eluant, affording 70 mg of yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09012487B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-dcc6b91e6c844c0b92ce1d042985eb23 |
| Source note | uspto-grants-2015_04 |