HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 67697967, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 1-Chloroethyl chloroformate | HCID 521305 | — |
| Reactant | HCID 45789390 | HCID 45789390 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67697967 | HCID 67697967 | — |
Reaction Steps
Combine 8-benzyl-1-(4-fluoro-phenyl)-1,3,8-triazaspiro[4.5]dec-2-en-4-one (10 mmol) and 1,2-dichloroethane (70 mL). Cool using an ice bath. Add in dropwise fashion, 1-chloroethyl chloroformate (48.6 mmol). Warm to ambient temperature and maintain for 1 h. Extract using saturated NaHCO3 (120 mL). Extract the aqueous phase using dichloromethane (120 mL). Combine the organic layers, extract with saturated NaCl, dry over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Add anhydrous methanol (70 mL) and heat at reflux for 1 h. Concentrate in in vacuo to obtain a residue and purify to obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05635510 |
| Source dataset | uspto-grants-1997_06 |
| ORD ID | ord-8242631a7698496d8d6d62138be7ca64 |
| Source note | uspto-grants-1997_06 |