HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Isobutyl 3-(Tert-Butyldisulfanyl)-1-(1-(Dichlorophosphoryl)Piperidin-4-ylamino)-1-Oxopropan-2-ylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Isobutyl 3-(Isopropyldisulfanyl)-1-Oxo-1-(Piperidin-4-ylamino)Propan-2-ylcarbamate | HCID 71572473 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Isobutyl 3-(Tert-Butyldisulfanyl)-1-(1-(Dichlorophosphoryl)Piperidin-4-ylamino)-1-Oxopropan-2-ylcarbamate | HCID 87108177 | — |
Reaction Steps
To the compound from Example 61 (7.746 g, 18.12 mmol) in DCM (200 ml) at −78° C. was slowly injected POCl3 (1.69 ml, 18.12 mmol) under Ar, followed by the addition of Et3N (7.58 ml, 54.36 mmol). The reaction was stirred at RT for 5 h, concentrated to remove excess base and solvent. The title compound was given as white solid after ISCO purification (50% EtAc/Hexane).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09278987B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-5ef87538a87f41009d9a52faaf1c9180 |
| Source note | uspto-grants-2016_03 |