반응 #709602

반응 방정식

hydrochloric acid

2-(3-methoxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride

trisodium phosphorothioate

→

2-(3-methoxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride

수율 77.0%

용매

water

반응 조건

후처리

1. 1
   온도the mixture was heated at 65° C. for 30 minutes
2. 2
   농축The resulting solution was concentrated under reduced pressure
3. 3
   workup.ADDITIONthe concentrate was mixed with 9.8 ml of isopropanol, insolubles
4. 4
   여과were filtered off
5. 5
   농축the filtrate was concentrated under reduced pressure
6. 6
   workup.ADDITIONEther was added to the concentrate
7. 7
   기타the crystals which separated out
8. 8
   여과were collected by filtration
9. 9
   기타reprecipitated from a mixture of ethanol and ether

실험 절차

1.77 g of trisodium phosphorothioate were added to an ice-cooled solution of 2.1 g of 2-(3-methoxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride in 12 ml of water, and the mixture was stirred at room temperature for about one hour. 9.8 ml of 1N hydrochloric acid were then added, and the mixture was heated at 65° C. for 30 minutes. The resulting solution was concentrated under reduced pressure, the concentrate was mixed with 9.8 ml of isopropanol, insolubles were filtered off, and the filtrate was concentrated under reduced pressure. Ether was added to the concentrate, and the crystals which separated out were collected by filtration and reprecipitated from a mixture of ethanol and ether, giving 1.6 g of 2-(3-methoxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride.

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