HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → 3-Bromo-6,7-dihydro-5H-pyrrolo[3,4-b]pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 3-Bromo-6-trityl-6,7-dihydro-5H-pyrrolo[3,4-b]pyridine | HCID 57753674 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 3-Bromo-6,7-dihydro-5H-pyrrolo[3,4-b]pyridine | HCID 57753562 | — |
Reaction Steps
To a cooled (0° C.) solution of 3-bromo-6-trityl-5,7-dihydropyrrolo[3,4-b]pyridine (1.57 g, 3.66 mmol) in chloroform (15 mL) and methanol (15 mL) was added trifluoroacetic acid (30 mL) over 1 min. On complete addition, the solution was stirred for 5 min then the cold bath removed and stirring continued for 30 min. This solution was concentrated under reduced pressure and the residue taken up in HCl (30 mL, 1M aq.). This mixture was extracted with ether (2×20 mL) then the aqueous phase basified with sodium hydroxide (5M aq.). This mixture was extracted with dichloromethane (3×20 mL). The combined dichloromethane extract was dried over magnesium sulfate and concentrated under reduced pressure to give the title compound as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403850B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-aa8fd62226e14a29a1ba28e1efd5b5ba |
| Source note | uspto-grants-2016_08 |