HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 66603835, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 66603654 | HCID 66603654 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66603835 | HCID 66603835 | 47.8% |
Reaction Steps
2.08 g of DIEA and then 1.745 g of ethyl chloroformate are added to a solution of 1.6 g of benzyl 4-{[4-({[(1,1-dimethylethoxy)carbonyl]amino}methyl)-2-(methoxycarbonyl)phenyl]amino}piperidine-1-carboxylate obtained in stage 5.2 in 11 ml of DCM. The mixture is stirred at AT for 4 days. It is evaporated under reduced pressure. The residue is taken up in 10 ml of pyridine (10 ml) and 0.7 g of ethyl chloroformate is added. The mixture is stirred at AT for 4 h 00. It is evaporated under reduced pressure. The residue is chromatographed on silica gel, elution being carried out with an AcOEt/heptane mixture, (10/90, v/v) as far as (30/70, v/v), to give 0.875 g of the expected product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846654B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-77f4e90549764ff0a130c58477d8f4b3 |
| Source note | uspto-grants-2014_09 |