HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 57587974, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 57587980 | HCID 57587980 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57587974 | HCID 57587974 | 66.4% |
Reaction Steps
(RS)-{Allyloxycarbonyl-[(4-chloro-phenyl)-phenyl-methyl]-amino}-acetic acid ethyl ester (18 g, 46.4 mmol) was dissolved in THF (60 mL), water (60 mL), and MeOH (60 mL) and treated with lithium hydroxide monohydrate (3.9 g, 92 mmol) at 20° C. for 2 h. The mixture was evaporated and extracted with AcOEt, 1 N HCl and 50% NaCl. The crude product was crystallized from heptane/ethyl acetate 10:1 (100 mL). One obtained 11.08 g (66%) of white crystals. MS: m/z=358 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07498339B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-d77408e7d6e04f77944eea3ea5207b47 |
| Source note | uspto-grants-2009_03 |