HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → HCID 86660456, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 49766392 | HCID 49766392 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86660456 | HCID 86660456 | 81% |
Reaction Steps
A flask is charged successively with 1 g (2.89 mmol) of 2-bromo-N-(2-(hydroxymethyl)-1H-pyrrolo[2,3-b]pyridin-5-yl)benzamide (Example 16), 100 mL of tetrahydrofuran and 408 μL (4.34 mmol) of phosphorus bromide (PBr3) under argon atmosphere. It is stirred at room temperature for 18 hours. The solvent is then evaporated under reduced pressure, and the residue is taken up in 150 mL of ethyl acetate. The organic phase is washed with 3×50 mL of water, dried over sodium sulphate and evaporated under reduced pressure. The precipitate obtained is dried under vacuum for 1 h, finally obtaining 957 mg of a brown solid (raw yield 81%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08580815B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-9c4eb020c91d4bd2b1dab8fce4a0c36b |
| Source note | uspto-grants-2013_11 |