HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 68796684, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodiumacetoxyborohydride | HCID 23670382 | — |
| Reactant | Methyl 5-amino-1H-pyrrolo[2,3-b]pyridine-2-carboxylate | HCID 40152010 | — |
| Reactant | HCID 87562064 | HCID 87562064 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 68796684 | HCID 68796684 | 10.1% |
Reaction Steps
A reactor is charged with 120 mg (0.34 mmol) of the solid obtained in step 2, 15 ml of anhydrous dichloromethane, 78 mg (0.41 mmol) of methyl 5-amino-1H-pyrrolo[2,3-b]pyridine-2-carboxylate, 216 mg (1.02 mmol) of sodium acetoxyborohydride and a catalytic amount of acetic acid. The mixture is stirred at room temperature for 24 hours. The solvent is then evaporated under reduced pressure and the residue is taken off in 100 ml of water. The aqueous phase is extracted by 3*30 ml ethyl acetate. The aqueous phases are combined, dried on sodium sulphate and then evaporated under reduced pressure. The raw product obtained is purified by preparative HPLC and 18 mg of a solid is obtained (10%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08580815B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-3c752877b3e74669990baba8a9b886c4 |
| Source note | uspto-grants-2013_11 |