1,4-Dibromo-2,3-butanediol → HCID 86752373, 화합물

HRID 481279

반응식

HRID 481279 반응식
Br[CH2:2][CH:3]([OH:8])[CH:4]([OH:7])[CH2:5]Br.[OH2:9].[OH2:10].O.O.O.O.O.O.O.O.O.O.[P:21]([O-:25])([O-:24])([O-:23])=[S:22].[Na+].[Na+].[Na+]>CN(C=O)C.O.[N+]([O-])([O-])=O.[Ag+]>[OH2:7].[OH2:23].[OH2:9].[OH2:7].[P:21](=[S:22])([OH:25])([OH:24])[OH:23].[P:21](=[S:22])([OH:25])([OH:24])[OH:23].[CH2:2]([OH:10])[C@H:3]([C@@H:4]([CH2:5][OH:9])[OH:7])[OH:8]

참가 물질

6

반응물 2

HCID 985121,4-Dibromo-2,3-butanediolHCID 45052183Sodium phosphorothioate hydrate (3:1:12)

생성물 1

HCID 86752373HCID 86752373, 화합물수율 285%

시약·촉매·용매 3

HCID 24470Silver Nitrate촉매HCID 962Water용매HCID 6228Dimethylformamide용매

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.

후처리

  1. customto precipitate excess sodium thiophosphate
  2. filtrationThe precipitate is filtered out
  3. customthe filtrate dried under high vacuum
  4. customThe solid residue is triturated with methanol
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-4dd8f3956e434e258e1ccf9a607920c0
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05789219

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