HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxybromide → 1-Bromo-4-hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxybromide | HCID 24613 | — |
| Reactant | 7-(4-Methoxy-phenoxy)-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester | HCID 66712618 | — |
| Reactant | HCID 178450860 | HCID 178450860 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1-Bromo-4-hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid | HCID 86014568 | — |
Reaction Steps
1,4-Dihydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester (Example D-1 d) Compound A) (29.0 g) and phosphorous oxybromide (67.5 g) in 600 ml anhydrous acetonitrile was stirred at reflux for 4 hours. After cooling the reaction mixture was concentrated and saturated sodium bicarbonate solution and ethyl acetate were added to the residue and stirred overnight. Precipitate that formed between layers was collected and washed with water to give the title compound (10.2 g). MS-(+)-ion M+1=376.0, 378.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916585B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-2f132e99368e43ce9b6ca195fb3b1493 |
| Source note | uspto-grants-2014_12 |