1,4-Dibromo-2,3-butanediol → HCID 86752373、化合物

HRID 1275415

反応式

HRID 1275415 の反応式
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]

参加物

6

反応物 2

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

生成物 1

HCID 86752373HCID 86752373、化合物収率 285%

試薬・触媒・溶媒 3

HCID 24470Silver Nitrate触媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2d5564b47fef4cd8bd37db7b1ab47034
出典データセット
uspto-grants-2000_12
特許番号
US06160153

関連ノート

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