HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68866398, compound → HCID 68863974, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68866398 | HCID 68866398 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68863974 | HCID 68863974 | 94.4% |
Reaction Steps
A solution of Example 275E (1.58 g) in 100 mL of ethyl acetate was hydrogenated under 60 psi pressure for 16 hours in the presence of 475 mg of 10% palladium on charcoal. The mixture was filtered, concentrated, treated with diethyl ether, and filtered. The filter cake was washed with diethyl ether to provide 1.5 g of the desired product as a mixture of R and S isomers. MS (ESI(+)) m/e 395 (M+NH4)+; MS (ESI(−)) m/e 376 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 9.91 (s, 1H), 7.61-7.71 (m, 2H), 7.40-7.46 (m, 1H), 7.31 (dt, 1H), 7.08 (d, 1H), 6.87 (d, 1H), 3.65 (s, 3H), 3.05-3.08 (m, 1H), 2.64-2.78 (m, 2H), 1.58-1.79 (m, 4H), 1.02 (d, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07491718B2 |
| Source dataset | uspto-grants-2009_02 |
| ORD ID | ord-4861589b34334f259dbe412a8a7ea507 |
| Source note | uspto-grants-2009_02 |