Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Carbonic acid-guanidine (1:1) | HCID 286947 | — |
| Reactant | Methyl 2-(4-(cyanomethyl)benzyl)-3-oxobutanoate | HCID 59590640 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178433372 | HCID 178433372 | — |
Reaction Steps
A stirred mixture of the crude product from step (i) and guanidine carbonate (36.7 g, 0.20 mol) in methanol (389 g) was heated under reflux for 7 hours. The mixture was cooled to 30° C., diluted with water (222 g), and the pH of the solution was adjusted to pH 6.5 with acetic acid. After the mixture was cooled to 5° C., the resulting precipitate was collected by filtration, washed with methanol twice (167 g, 333 g), and dried under reduced pressure to give the subtitle compound as a solid, 32.6 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08476288B2 |
|---|
| Source dataset | uspto-grants-2013_07 |
|---|
| ORD ID | ord-7c417083a22c462e8fcf15d1827633ac |
|---|
| Source note | uspto-grants-2013_07 |
|---|
