HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 22903480, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 22903479 | HCID 22903479 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22903480 | HCID 22903480 | — |
Reaction Steps
To a solution of 7-chloro-1-{6-[2-(2-hydroxyethoxy)benzoylamino]nicotinoyl}-2,3,4,5-tetrahydro-1H-benzazepine (0.5 g )in pyridine (10 ml) is added with stirring methanesulfonyl chloride (0.1 ml) under ice-cooling, and the mixture is stirred at room temperature for 2 hours. To the reaction solution is added water, and the precipitated crystals are collected by filtration, and dissolved in dichloromethane. The mixture is washed successively with diluted hydrochloric acid and water, dried over magnesium sulfate and evaporated under reduced pressure. The residue is crystallized from diethyl ether to give 7-chloro-1-{6-[2-(2-methanesulfonyloxyethoxy)benzoylamino]nicotinoyl}-2,3,4,5-tetrahydro-1H-benzazepine (0.59 g) as white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05677299 |
| Source dataset | uspto-grants-1997_10 |
| ORD ID | ord-a36c8e5b0bc34f77bf07100b5c0e416d |
| Source note | uspto-grants-1997_10 |