반응 #1362597

ord-2d5564b47fef4cd8bd37db7b1ab47034

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타to precipitate excess sodium thiophosphate
  2. 2
    여과The precipitate is filtered out
  3. 3
    기타the filtrate dried under high vacuum
  4. 4
    기타The solid residue is triturated with methanol
  5. 5
    여과filtered

실험 절차

A solution of 1,4-dibromo-2,3-butanediol (1.0 g, 4.0 mmol) in 5 ml DMF is added to sodium thiophosphate dodecahydrate (3.8 gm, 10.1 mmol) in 20 ml H2O. The mixture is stirred overnight at room temperature. A 5% silver nitrate solution is added to precipitate excess sodium thiophosphate. The precipitate is filtered out and the filtrate dried under high vacuum. The solid residue is triturated with methanol and filtered to yield 1.8 g (3.8 mmol) of threitol bis-phosphorothioate tetrahydrate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06160153uspto-grants-2000_12