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

HRID 1598393

반응식

HRID 1598393 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 thiophosphate dodecahydrate

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-d8912c5171b5473da905689e586426fe
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05736624

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