HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Chloroethyl chloroformate → HCID 22174822, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Chloroethyl chloroformate | HCID 521305 | — |
| Reactant | HCID 22174832 | HCID 22174832 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 22174822 | HCID 22174822 | 63% |
Reaction Steps
A solution of 1-phenylsulfonyl-4-(4-benzylpiperazin-1-yl)-1H-indazole (433 mg, 1.0 mmol) in 1,2-dichloroethane is treated with 1-chloroethyl chloroformate (0.27 mL, 2.5 mmol) heated at reflux temperature for 2 hr, and concentrated in vacuo. The resultant residue is heated at reflux temperature in methanol for 1.5 hr, cooled, concentrated in vacuo and reconcentrated from ether. The resulting tan solid is triturated with ether and crystallized from hot ethanol to give the title compound as a tan solid 237 mg (63% yield), mp 203-205° C., identified by HNMR and mass spectral analyses.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07541370B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-425639cd16d149529e8789414f78083b |
| Source note | uspto-grants-2009_06 |