反应详情

945 mg of trisodium phosphorothioate were added to a solution of 1.05 g of 2-(3-hydroxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride in 6.4 ml of water, cooled with ice-water, and the mixture was stirred at room temperature for about one hour. 5.2 ml of 1N hydrochloric acid were added, and the mixture was heated at 65° C. for 30 minutes and then concentrated under reduced pressure. The concentrate was mixed with 5.2 ml of methanol, insolubles were filtered off, and the filtrate was concentrated under reduced pressure. Anhydrous ether was added to the concentrate, and the precipitated crystals were collected by filtration and washed with ether, giving 670 mg of 2-(3-hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride.

1. temperaturethe mixture was heated at 65° C. for 30 minutes
2. concentrationconcentrated under reduced pressure
3. additionThe concentrate was mixed with 5.2 ml of methanol, insolubles
4. filtrationwere filtered off
5. concentrationthe filtrate was concentrated under reduced pressure
6. additionAnhydrous ether was added to the concentrate
7. filtrationthe precipitated crystals were collected by filtration
8. washwashed with ether