HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 12846663, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,5-Diazabicyclo(4.3.0)non-5-ene | HCID 76349 | — |
| Reactant | HCID 15578367 | HCID 15578367 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 12846663 | HCID 12846663 | — |
Reaction Steps
1,5-Diazabicyclo[4.3.0]non-5-ene (3.2 g) was added dropwise to a stirred solution of ethyl 5,6-dibromo-2,4-dioxo-6-(4-methoxyphenyl)hexanoate (5.6 g) in dimethylsulphoxide (30 ml) maintained at a temperature of 15°-20° C. After 30 minutes at room temperature, water (50 ml) and petroleum ether 40°-60° C. (20 ml) were added with cooling. The yellow solid which precipitated was filtered off and recrystallised from ethanol-water. A second recrystallisation from ethyl acetate-petroleum ether 60°-80° C. yielded the title product as yellow needles (mp 131°-133° C. with sublimation).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04304728 |
| Source dataset | uspto-grants-1981_12 |
| ORD ID | ord-4d85b482de7c4fa49c3ae377c5af7d98 |
| Source note | uspto-grants-1981_12 |