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Sodium Hydroxide → 3-Amino-2,2,4,4-tetramethylthietan-1,1-dioxide

HRID 1262976
ノート
印刷プレビュー

反応式

HRID 1262976 の反応式
[NH2:1][CH:2]1[C:5]([CH3:7])([CH3:6])[S:4][C:3]1([CH3:9])[CH3:8].[O-:10]I(=O)(=O)=O.[Na+].[OH-:16].[Na+]>O>[NH2:1][CH:2]1[C:5]([CH3:7])([CH3:6])[S:4](=[O:10])(=[O:16])[C:3]1([CH3:9])[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 115210993-Amino-2,2,4,4-tetramethylthietaneHCID 23667635Sodium periodate

生成物 1

HCID 137335683-Amino-2,2,4,4-tetramethylthietan-1,1-dioxide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 14.53 g. (0.1 mole) 3-amino-2,2,4,4-tetramethylthietane and 64.17 g. (0.3 mole) sodium m-periodate in 500 ml. water was stirred overnight at room temperature. The reaction mixture was adjusted to pH 13 with sodium hydroxide solution and the precipitated sodium iodate removed by filtration. The filtrate was washed with 100 ml. ethyl ether, the aqueous phase extracted continuously with methylene chloride over 18 hours, the extract dried (MgSO4) and solvent evaporated in vacuo. The residual solid was recrystallized from ethyl acetate to provide 8.5 g. of product, M.P. 104°-106.5° C. A second crop of crystals was obtained, 2.7 g., M.P. 103°-106° C. Total yield, 63%.

後処理

  1. customthe precipitated sodium iodate removed by filtration
  2. washThe filtrate was washed with 100 ml
  3. extractionethyl ether, the aqueous phase extracted continuously with methylene chloride over 18 hours
  4. dry with materialthe extract dried (MgSO4) and solvent
  5. customevaporated in vacuo
  6. customThe residual solid was recrystallized from ethyl acetate
  7. customto provide 8.5 g
  8. customA second crop of crystals was obtained

出典と根拠

ORDレコード
ord-541f6130e36b430d9caca9959ec00a1c
出典データセット
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04454328

反応ノート

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