HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → (R)-3-{4-[(4-tert-butylphenylamino)methyl]benzoylamino}-2-hydroxypropionic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 4-Tert-Butylaniline | HCID 69861 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | (R)-3-(4-Formylbenzoylamino)-2-hydroxypropionic acid | HCID 86586064 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Trimethyl orthoformate | HCID 9005 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | (R)-3-{4-[(4-tert-butylphenylamino)methyl]benzoylamino}-2-hydroxypropionic acid | HCID 69733516 | — |
Reaction Steps
The above resin bound (R)-3-(4-formylbenzoylamino)-2-hydroxypropionic acid was treated with a 0.5 M solution of 4-tert-butylaniline (0.25 mmol) in a mixture of N-methyl-2-pyrrolidinone and trimethylorthoformate (1:1, 0.5 mL) and glacial acetic acid (50 μL) for 1 hour at 25° C. Sodium cyanoborohydride (250 μmol, 16 mg) dissolved in a mixture of N-methyl-2-pyrrolidinone and methanol (1:1, 0.25 mL) was added and the mixture was vortexed at 25° C. for 4 hours followed by filtration and washing with a mixture of N-methyl-2-pyrrolidinone and methanol (1:1, 2×1 mL) 3×1 mL N-methyl-2-pyrrolidinone (3×1 mL) and a mixture of 1,2-dichloropropane and diisopropylethylamine (7:1, 2×0.75 mL).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06953812B2 |
| Source dataset | uspto-grants-2005_10 |
| ORD ID | ord-b5a2198e6cbc46909f87db4ea88f8bf4 |
| Source note | uspto-grants-2005_10 |