HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 135719064, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Formamidine acetate | HCID 160693 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 86591733 | HCID 86591733 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 135719064 | HCID 135719064 | 27.4% |
Reaction Steps
To a mixture of 2-fluoro-3-(1-(4-fluorobenzyl)-5-methanesulfonyl-1H-pyrrolo[2,3-b]pyridin-2-yl)-3-oxopropionic acid ethyl ester obtained in Example 36 (3) (88 mg), formamidine acetate (42 mg) and methanol (1.2 ml), sodium methoxide (0.6 ml, 1 mol/l solution in methanol) was added at 15 to 30° C. and the mixture was stirred at the same temperature for 18 hours. The mixture was neutralized with acetic acid and diluted with ethyl acetate. The organic layer was washed with water, dried and concentrated under reduced pressure. The resulting residue was separated using silica gel column chromatography (methanol:dichloromethane=5:95) to obtain the desired product (23 mg) in a white amorphous form.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06673797B1 |
| Source dataset | uspto-grants-2004_01 |
| ORD ID | ord-10495842cdbe4bb1a9d5c97fc0c415e9 |
| Source note | uspto-grants-2004_01 |