HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl acetoacetate → HCID 59272686, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl acetoacetate | HCID 7757 | — |
| Reactant | 2-Chloro-4-fluorobenzaldehyde | HCID 145024 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 67500107 | HCID 67500107 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59272686 | HCID 59272686 | 31.6% |
Reaction Steps
2 mmol 4-methyl-5-thiazolformamidine acetate, 2 mmol 2-chloro-4-fluorobenzaldehyde, 2 mmol methyl acetoacetate and 2.2 mmol sodium acetate were reacted under reflux in 10 ml anhydrous ethanol for 20 hr, concentrated, and then ethyl acetate and water were added to separate the layers. The ethyl acetate layer was dried over anhydrous sodium sulfate, and separated by a column chromatography to obtain 0.24 g of a colorless crystal with mp 145-147° C.; 1H-NMR (400 MHz, DMSO-d6) δ 2.34 (3H, s); 2.38 (3H, s); 3.50 (3H, s); 5.95 (1H, s); 7.12-7.49 (3H, m); 9.08 (1H, s); 9.61 (1H, s); MS (EI) 379.0 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08168642B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-86967fb6dba84520ae0926421b35db35 |
| Source note | uspto-grants-2012_05 |