HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86758362, compound → HCID 18467805, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86758362 | HCID 86758362 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 18467805 | HCID 18467805 | 93.8% |
Reaction Steps
2,5-Dimethyl-3-methoxycarbonylmethylene-2-tetrahydrofuroic acid, t-butyl ester (28 mg, obtained from Step A) was dissolved in 0.25 mL of ethyl acetate and 0.25 mL of methanol. This mixture was hydrogenated under a balloon of hydrogen at room temperature for 1.25 h. The reaction mixture was filtered over a pad of celite, and the crude product obtained after removal of volatiles was purified via a silica gel SepPak, providing 21 mg of the desired compound cleanly (75% yield), homogeneous by TLC (Rf=0.2 in 10/1 hexane/ethyl acetate)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06420418B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-1e5a2b6a049b4681b663d852fd9fdc6b |
| Source note | uspto-grants-2002_07 |