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Sodium hydrosulfide hydrate → Sodium 2-hydroxy-3-sulfanylpropane-1-sulfonate

HRID 1275416
ノート
印刷プレビュー

反応式

HRID 1275416 の反応式
O.Cl[CH2:3][CH:4]([OH:10])[CH2:5][S:6]([O-:9])(=[O:8])=[O:7].[Na+:11].O.[SH-:13].[Na+]>CN(C=O)C>[SH:13][CH2:3][CH:4]([OH:10])[CH2:5][S:6]([O-:9])(=[O:8])=[O:7].[Na+:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 16211346Sodium hydrosulfide hydrateHCID 23665651Sodium 3-chloro-2-hydroxypropane-1-sulfonate--water (1/1/1)

生成物 1

HCID 23663670Sodium 2-hydroxy-3-sulfanylpropane-1-sulfonate収率 172.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To sodium 3-chloro-2-hydroxypropanesulfonate hydrate (2.0 g), sodium hydrosulfide hydrate (0.42 g) was added in 10 mL DMF. The mixture was refluxed overnight. When the reaction mixture was cooled down, white solid was isolated, rinsed with ether and acetone to obtain 1.9 g crude sodium 3-mercapto-2-hydroxypropane sulfonate. The crude product was dissolved in water and preferentially precipitated the desired product by adding acetone. The precipitated product was then filtered and dried under vacuum to get 1.04 g of the title compound.

後処理

  1. temperatureThe mixture was refluxed overnight
  2. temperatureWhen the reaction mixture was cooled down
  3. customwhite solid was isolated
  4. washrinsed with ether and acetone

出典と根拠

ORDレコード
ord-dba88060dfeb4f4c8d98aa631c8a672c
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06160167

反応ノート

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