HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 178497018, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 178501028 | HCID 178501028 | — |
| Catalyst | Manganese dioxide | HCID 14801 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178497018 | HCID 178497018 | — |
Reaction Steps
A mixture of 59.9 g methyl (6S)-4,5,6,7-tetrahydro-imidazo[4,5-c]pyridine-6-carboxylate and 172.5 g MnO2 in 2 l anhydrous 1,4-dioxane is refluxed for 4 hours. The reaction mixture is allowed to come to 60-70° C. whereupon 1 l methanol is slowly added. The suspension is filtered hot and the filtrate is concentrated under reduced pressure to give a first batch of the title product. The filter cake is washed with hot methanol (2 l) and concentrated under reduced pressure to a volume of about 50 ml. 80 ml 1,4-dioxane is added whereupon precipitation takes place. After filtration a second batch of the title product is obtained. The washing procedure of the initial filter cakes is repeated once again to give a third batch of the title product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08273890B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-c63c0bbab4264c0cbfcc59b711893fa0 |
| Source note | uspto-grants-2012_09 |