HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfate → HCID 67496094, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | 2-Amino-5-bromobenzoic acid | HCID 79858 | — |
| Reactant | Tetrahydro-4H-pyran-4-one | HCID 121599 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 67496094 | HCID 67496094 | 48.2% |
Reaction Steps
A mixture of 5 g of 2-amino-5-bromobenzoic acid, 9.27 g of tetrahydro-4H-pyran-4-one and 32 g of Na2SO4 in 50 ml of acetic acid is stirred overnight at room temperature. The reaction mixture is filtered. A further 9.27 g of tetrahydro-4H-pyran-4-one and 32 g of Na2SO4 are added and the resulting mixture is stirred overnight at room temperature. This mixture is filtered and 9.81 g of NaBH(OAc)3 are added. The resulting mixture is allowed to cool to room temperature over 2 hours. The reaction medium is evaporated under reduced pressure and the residue is taken up in EtOAc. It is washed with aqueous 1N HCl solution. The organic phase is dried over Na2SO4, filtered and evaporated under reduced pressure to give 3.35 g of the expected product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722659B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-4f1a2a208a6447678a7e1b4cd9ca8f3c |
| Source note | uspto-grants-2014_05 |