반응 #709593

반응 방정식

trisodium phosphorothioate

2-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylchloride hydrochloride

hydrochloric acid

→

2-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylmercaptan hydrochloride

수율 104.3%

용매

water

—

ice water

반응 조건

후처리

1. 1
   온도the mixture was heated to 50° C. for 30 minutes
2. 2
   workup.DISTILLATIONthe solvent was then distilled off under reduced pressure
3. 3
   workup.ADDITIONThe concentrate was mixed with 8 ml of methanol, insolubles
4. 4
   여과were filtered off
5. 5
   농축the filtrate was concentrated under reduced pressure
6. 6
   기타The concentrate was crystallized
7. 7
   workup.ADDITIONby adding ether
8. 8
   여과the crystals were collected by filtration
9. 9
   세척washed with ether

실험 절차

0.945 g of trisodium phosphorothioate were added to a solution of 1.21 g of 2-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylchloride hydrochloride in 8 ml of water, kept cooled in ice-water, and the mixture was stirred for about 3 hours at room temperature. After adding 6 ml of 1N hydrochloric acid, the mixture was heated to 50° C. for 30 minutes, and the solvent was then distilled off under reduced pressure. The concentrate was mixed with 8 ml of methanol, insolubles were filtered off, and the filtrate was concentrated under reduced pressure. The concentrate was crystallized by adding ether, and the crystals were collected by filtration and washed with ether, giving 1.25 g of 2-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylmercaptan hydrochloride.

출처