HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 57297845, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 1-Methoxy-3-trimethylsilyloxy-1,3-butadiene | HCID 101051 | — |
| Reactant | HCID 11030982 | HCID 11030982 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 57297845 | HCID 57297845 | 65% |
Reaction Steps
A mixture of 1-methoxy-3-trimethylsilyloxy butadiene (776 mg, 4.51 mmol) and methyl (5,8-dioxo-3,4,5,8-tetrahydrobenzo [2,3-C] pyran-3-yl) ketone (309 mg, 1.50 mmol) in 6 mL of dry toluene was stirred for 90 minutes at room temperature under argon atmosphere. The solvent was then removed in vacuo and the dried residue was dissolved in 10 mL of THF. To this solution was added 2 mL of a 4% aq. HCl solution. The combined organic layers were then washed with water and dried over MgSO4. Flash chromatography (toluene:ethyl acetate; 95%:5%) of the residue gave 180 mg (65% yield) of the titled compound (MP: 169°-170° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05606037 |
| Source dataset | uspto-grants-1997_02 |
| ORD ID | ord-415e6bc54cb74f10acb61d6c67e2a0c0 |
| Source note | uspto-grants-1997_02 |