HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22483528, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 19598479 | HCID 19598479 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Product | HCID 22483528 | HCID 22483528 | 78.5% |
Reaction Steps
10 g of palladium on carbon at 5% by weight and containing 50% water were added to a solution of 19.3 g of 4-oxo-4,5,6,7-tetrahydro-1-N-(β-hydroxypropyl)indole, obtained in the preceding stage, in 300 cm3 of diglyme. The temperature of the reaction medium was raised to the reflux temperature of diglyme for 5 hours, after removing the water by azeotropy. The catalyst was then filtered off on celite and then the diglyme was evaporated off. 17 g of crude product were obtained. After chromatography on silica gel (heptane/ethyl acetate=1/4), 15 g of viscous product were obtained, which product was crystallized by the addition of 15 cm3 of dichloromethane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05869692 |
| Source dataset | uspto-grants-1999_02 |
| ORD ID | ord-d2d6072420294d2fa4086aa51f09f08f |
| Source note | uspto-grants-1999_02 |