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

HRID 1598393

反応式

HRID 1598393 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 thiophosphate dodecahydrate

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-d8912c5171b5473da905689e586426fe
出典データセット
uspto-grants-1998_04
特許番号
US05736624

関連ノート

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