HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperidin-4-ol → 1-(12-Chloro-6,6-dioxo-5,6-dihydro-6lambda*6*-thia-4,5-diaza-chrysen-9-yl)-piperidin-4-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperidin-4-ol | HCID 79341 | — |
| Reactant | 12-Chloro-9-fluoro-5H-6-thia-4,5-diaza-chrysene 6,6-dioxide | HCID 68183182 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | 1-(12-Chloro-6,6-dioxo-5,6-dihydro-6lambda*6*-thia-4,5-diaza-chrysen-9-yl)-piperidin-4-ol | HCID 68183218 | 48.1% |
Reaction Steps
12-Chloro-9-fluoro-5H-6-thia-4,5-diaza-chrysene 6,6-dioxide 503 (100 mg, 0.3 mmol), 4-hydroxy piperidine (121 mg, 1.2 mmol) and NMP (2 ml) were heated in microwave at 180° C. for 4 h. After cooling, the mixture was poured into ice cold water and the resulting precipitate was collected by filtration and dried. The crude residue was purified by column chromatography with DCM/MeOH (99:1) as the eluent to give the title compound (60 mg, 48%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09102688B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-820b995beeac4948aed292c5fb805e50 |
| Source note | uspto-grants-2015_08 |