HuagongsheHuagongshe Chemistry Print Report · For research reference only
Disodium disulfite → HCID 136236986, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Disodium disulfite | HCID 24346 | — |
| Reactant | 2-Amino-5-fluorobenzamide | HCID 10241003 | — |
| Reactant | HCID 118272349 | HCID 118272349 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 136236986 | HCID 136236986 | — |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
A suspension of 2-amino-5-fluorobenzamide (135 mg, 0.88 mmol), 1-(4-[1,3]dioxolan-2-yl-phenyl)-cyclopentanol (206 mg, 0.88 mmol) and sodium disulfite (170 mg, 0.89 mmol) in N,N-dimethylacetamide (2 ml) is heated to 150° C. and stirred at this temperature for 3 hours. The reaction mixture is allowed to reach room temperature and poured into ice water. The resulting precipitate is collected by filtration and washed with water. It is chromatographed on a silica gel column with methanol/dichloromethane as eluent to afford 6-fluoro-2-[4-(1-hydroxy-cyclopentyl)-phenyl]-3H-quinazolin-4-one as white solid; HPLC/MS 1.80 min (A), [M+H] 325;
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09388142B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-364b86a8df2e405b91196eea50074bc8 |
| Source note | uspto-grants-2016_07 |