HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethylamine → HCID 86718855, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | HCID 86718854 | HCID 86718854 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86718855 | HCID 86718855 | 70.5% |
Reaction Steps
In a round-bottomed flask, the above prepared {(S)-1-[(S)-1-(4-hydroxymethyl-phenylcarbamoyl)-pentylcarbamoyl]-2-phenyl-ethyl}-carbamic acid 9H-fluoren-9-ylmethyl ester (4.738 g, 7.822 mmol, Eq: 1.0) was dissolved in CH2Cl2 (28 ml). At 0°, diethylamine (28 ml, 19.80 g, 271 mmol, Eq: 35) was added and the reaction mixture stirred at ambient temperature overnight. All volatiles were evaporated i. V.; ensuing flash chromatography SiO2/CH2Cl2/10% MeOH, followed by crystallization from AcOEt, yielded 2.116 g of the title compound as light brown crystals. MS (ISP): (M+H) 384.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09301990B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-a1ede700267d439bbe7107861eaec30b |
| Source note | uspto-grants-2016_04 |