HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Methyl 4-methoxy-2-acetonyl-2-methylacetoacetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Chloroacetone | HCID 6571 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 4-methoxy-2-methylacetoacetate | HCID 11084163 | — |
| Catalyst | Benzyl triethylammonium chloride | HCID 66133 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Methyl 4-methoxy-2-acetonyl-2-methylacetoacetate | HCID 19871657 | 38.4% |
Reaction Steps
1.66 g (12 mmol) of potassium carbonate and 0.04 g (0.2 mmol) of benzyltriethylammonium chloride are suspended in 5 ml of acetonitrile. While stirring there are added thereto 1.60 g (10 mmol) of methyl 4-methoxy-2-methylacetoacetate and there are then added dropwise thereto within 15 minutes 1.39 g (15 mmol) of chloroacetone. The mixture is stirred at 20°-25° C. for a further 21 hours. The reaction mixture is poured into 20 ml of 2N HCl (pH value=1) and extracted 3 times with 20 ml of ethyl acetate each time. The combined organic phases are dried over sodium sulphate and evaporated on a rotary evaporator. The crude product distils at 95° C./0.03 mbar. There results 0.83 g (38.4%) of methyl 4-methoxy-2-acetonyl-2-methylacetoacetate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04892966 |
| Source dataset | uspto-grants-1990_01 |
| ORD ID | ord-f1f5cb04d72e48e881240abdc0ad3af2 |
| Source note | uspto-grants-1990_01 |