HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66855424, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Cyclobutanol | HCID 76218 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | Benzyl piperazine-1-carboxylate | HCID 643495 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66855424 | HCID 66855424 | — |
Reaction Steps
To a solution of 2.6 g triphosgene and 1.7 ml cyclobutanol in 40 ml dichloromethane were added 6.2 ml triethylamine dropwise at 0° C. After 30 minutes 4.4 ml benzyl 1-piperazinecarboxylate and 3.2 ml triethylamine were added at 0° C. The reaction mixture was allowed to warm to RT for 16 h. Excess triphosgene was destroyed by adding a solution of 2 g NaOH in 200 ml water and stirring for 2 h. The layers were separated, the organic layer dried over MgSO4 and concentrated. The crude product thus obtained was purified by chromatography on silica using heptane/ethyl acetate 4/1 to 2/1 as eluent. Yield: 5.9 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08669266B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-02ef5fdaf9c449a4b2f00ce7d84d603e |
| Source note | uspto-grants-2014_03 |