HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → (S)-2-(1-Cyano-4-hydroxyisoquinoline-3-carboxamido)propanoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | L-Alanine | HCID 5950 | — |
| Reactant | 1-Cyano-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester | HCID 67110122 | — |
| Reactant | HCID 178418582 | HCID 178418582 | — |
| Product | (S)-2-(1-Cyano-4-hydroxyisoquinoline-3-carboxamido)propanoic acid | HCID 24779987 | 70.8% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
A mixture of 1-cyano-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester (135 mg, 0.5 mmol, see Example 1(a)), (S)-alanine (225 mg, 2.5 mmol) and a 0.5 N solution of MeONa in methanol (5 mL, 2.5 mmol) was heated in a microwave oven with stirring for 40 min at 120° C. before the mixture was concentrated in vacuo. To the residue was added water (10 mL) and the mixture was washed with diethyl ether (4×40 mL). The pH of the purified solution was adjusted to about 2 by the addition of aqueous 6 N HCl. The resulting suspension was extracted with ethyl acetate (1×40 mL). The organic phase was dried over MgSO4 and concentrated in vacuo to give the title compound as a yellowish solid (101 mg); MS-(−)-ion: M−1=284.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928120B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-eb8c633f3ba641658e1be0dd79b5b182 |
| Source note | uspto-grants-2011_04 |