HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 68588340, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | HCID 22288339 | HCID 22288339 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68588340 | HCID 68588340 | — |
Reaction Steps
4.8 g (42.0 mmol) [1,4]diazepin-5-one are dissolved in 60 ml DCM and at ice bath temperature successively combined with 11.0 ml (83.9 mmol) triethylamine and 6.8 ml (46.2 mmol) benzyl chloroformate. The mixture is heated to RT and kept for three hours at this temperature. Then the mixture is concentrated and combined with water. The aqueous phase is extracted three times with ethyl acetate. The combined organic phases are dried on sodium sulphate, filtered and evaporated down i. vac. The crude product is [purified] by column chromatography on silica gel (eluant DCM/MeOH 95:5→90:10).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08309542B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-64ea7020a94548d4997eccf03ba194a8 |
| Source note | uspto-grants-2012_11 |