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Sodium borohydride → 3-Mercapto-2,2-dimethyl-1-propylsulfonamide

HRID 465934
ノート
印刷プレビュー

反応式

HRID 465934 の反応式
[S:1]([CH2:4][C:5]([CH3:12])([CH3:11])[CH2:6][S:7]([NH2:10])(=[O:9])=[O:8])C#N.[BH4-].[Na+]>C(O)C>[SH:1][CH2:4][C:5]([CH3:12])([CH3:11])[CH2:6][S:7]([NH2:10])(=[O:9])=[O:8]
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 4311764Sodium borohydrideHCID 104430543-Thiocyanato-2,2-dimethyl-1-propanesulfonamide

生成物 1

HCID 104649823-Mercapto-2,2-dimethyl-1-propylsulfonamide収率 16.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 5.15 g of 3-thiocyanato-2,2-dimethyl-1-propanesulfonamide in 100 ml of ethanol was little by little added 0.79 g of sodium borohydride with stirring and nitrogen gas atmosphere, taking an hour. The reaction mixture was refluxed for an hour and concentrated under reduced pressure. To the residue were added 20 ml of water and 30 ml of 1N-hydrochloric acid. The organic layer was collected, and the aqueous layer was washed with ethyl acetate (50 ml×3). The combined organic layers were dried over anhydrous magnesium sulfate and distilled to remove the solvent. The residue was subjected to a silica gel chromatography, eluting with chloroform-methanol (10:1), to obtain 0.76 g of 3-mercapto-2,2,-dimethyl-1-propanesulfonamide.

後処理

  1. waitnitrogen gas atmosphere, taking an hour
  2. temperatureThe reaction mixture was refluxed for an hour
  3. concentrationconcentrated under reduced pressure
  4. additionTo the residue were added 20 ml of water and 30 ml of 1N-hydrochloric acid
  5. customThe organic layer was collected
  6. washthe aqueous layer was washed with ethyl acetate (50 ml×3)
  7. dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
  8. distillationdistilled
  9. customto remove the solvent
  10. washeluting with chloroform-methanol (10:1)

出典と根拠

ORDレコード
ord-5778056959174b35918d0187a4a3f5dd
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05155108

反応ノート

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