HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethylamine → HCID 67321271, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | HCID 67320233 | HCID 67320233 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67321271 | HCID 67321271 | — |
Reaction Steps
A solution of 3.66 g (6.78 mmol) of 9H-fluoren-9-yl methyl((9S,12R)-9-isopropyl-11-oxo-2,7-dioxa-10-azabicyclo[12.2.2]octadeca-1(17),4,14(18),15-tetraen-12-yl)carbamate (1-1D) in 300 ml of dichloromethane was mixed with 75 ml of diethylamine and stirred at RT for 5 h. The mixture was concentrated and purified by preparative HPLC. Acetonitrile was removed from the combined product fractions in a rotary evaporator, saturated NaHCO3 solution was added, and the mixture was extracted twice with ethyl acetate, saturated with sodium chloride and again extracted with ethyl acetate. The combined ethyl acetate phases were dried over Na2SO4, filtered and concentrated. The resulting substance was pure enough for further reactions.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722655B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-72c568ad56ca4229bb8e44e7c19e0e3e |
| Source note | uspto-grants-2014_05 |