HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen chloride-ethyl acetate → HCID 66638003, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | HCID 66637482 | HCID 66637482 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66638003 | HCID 66638003 | 86.8% |
Reaction Steps
To the solution of thus obtained N-t-butoxycarbonyl-β-cyclohexyl-L-alanyl-glycyl-glycine ethy lester (506.2 mg, 1.22 mmol) in ethyl acetate (1 mL) under ice-cold condition, add 4M hydrogen chloride/ethyl acetate (3.0 mL, 12 mmol) with stirring, and then the reaction mixture was stirred for 4.5 hours at room temperature. Diethylether (12 mL) was added and the mixture was stirred under ice-cold condition, then the precipitate was collected by filtration to obtain hygroscopic crude crystals. The crude crystals were suspended in diethylether (10 mL)and collected by filtration to obtain β-cyclohexyl-L-alanyl-glycyl-glycine ethyl ester hydrochloride (370.3 mg) as colorless crystalline powder (yield 86%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08133864B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-6f31f8301fd74736977c014c3314cb3d |
| Source note | uspto-grants-2012_03 |