HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178433372, compound
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 (128.1 g) in methanol (915 mL) was heated under reflux for 5 hours. The mixture was cooled to room temperature, diluted with water (923 mL) and nuetralised with acetic acid. The mixture was then cooled to 10° C. and the resulting precipitate collected by filtration, washed with methanol (501 mL) and dried under reduced pressure to give the subtitle compound as a solid, 82.4 g; 1H NMR DMSO-d6: δ 10.91 (brs, 1H), 7.20-7.17 (m, 4H), 6.38 (s, 2H), 3.95 (s, 2H), 3.63 (s, 2H), 2.00 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476288B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-4f38c4a77d644a94bd290e0589827f9b |
| Source note | uspto-grants-2013_07 |