HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 7299381, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 7237625 | HCID 7237625 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 7299381 | HCID 7299381 | — |
Reaction Steps
N-(Benzyloxycarbonyl)-D-leucyl-L-leucine methyl ester (Example 29A, 1.12 g, 2.85 mmol) is provided at 0° C. in THF/water 2:1 (15 ml) and then lithium hydroxide monohydrate (140 mg, 5.71 mmol, 2 equivalents) is added. When the HPLC chromatogram (Method 2) shows complete conversion (about 1 h), the reaction mixture is adjusted to pH 3-4 with acetic acid, concentrated in vacuo under cold conditions and then freed of solvent by freeze-drying overnight. The crude product is purified by means of preparative HPLC (Method 13) whereby 958 mg (88.7% of theory) of the title compound are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07718611B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-15c99cdeca3947ddbfab9fe067cd5e7c |
| Source note | uspto-grants-2010_05 |