HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 22121894, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 4-Methylisoquinoline-5-sulfonyl chloride | HCID 15487110 | — |
| Reactant | HCID 22121941 | HCID 22121941 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 22121894 | HCID 22121894 | 54.4% |
Reaction Steps
To a suspension of 1.5 g of 2,7-dimethyl-hexahydro-1H-1,4-diazepine hydrobromide obtained in Reference Example 3 in 30 ml of pyridine was added 1.58 g of 1,8-diazabicyclo[5.4.0]-7-undecene, and after addition of 0.84 g of 5-chlorosulfonyl-4-methyl-isoquinoline, the mixture was stirred at room temperature for 1 hour. This reaction mixture was concentrated and the residue was diluted with water, extracted with chloroform, dried, and concentrated. The residue was purified by silica gel column chromatography (chloroform/methanol=30/1) and converted to the hydrochloride in the routine manner to provide 0.70 g of the objective compound (white crystals).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06153608 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-6ab3c4db7cd3464296d4875bb033a753 |
| Source note | uspto-grants-2000_11 |