HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenepropanoic acid, 4-methoxy-beta-oxo-, ethyl ester → Ethyl 2-(4-methoxybenzoyl)-3-(1,3-benzodioxol-5-yl)-4-nitro-butanoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenepropanoic acid, 4-methoxy-beta-oxo-, ethyl ester | HCID 76150 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 5-(2-Nitroethenyl)-1,3-benzodioxole | HCID 94945 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Ethyl 2-(4-methoxybenzoyl)-3-(1,3-benzodioxol-5-yl)-4-nitro-butanoate | HCID 10811775 | — |
Reaction Steps
Into a 45-L stirred reactor at ambient temperature were charged 5.819 kg (30.1 moles) 3,4-methylenedioxy-1-(2-nitroethenyl)-benzene and 24 L ethyl acetate. A solution of 5.355 kg (24.1 moles) ethyl 3-(4-methoxyphenyl)-3-oxopropionate in 16 L ethyl acetate was added. 280 g (275 ml, 1.84 moles) of 1,8-diaza-bicyclo[5.4.0]undec-7-ene in four equal portions was added over a 2.5 hour period. The reaction mixture was filtered through dicalite and the resulting filtered solution was used in the next step without any further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06946481B1 |
| Source dataset | uspto-grants-2005_09 |
| ORD ID | ord-f680ba6d1ae8483d9b0d419e5d5fd3da |
| Source note | uspto-grants-2005_09 |