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Water → HCID 13712178、化合物

HRID 414048
ノート
印刷プレビュー

反応式

HRID 414048 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:12][NH:13][CH2:14][CH2:15][NH:16][CH3:17].C(=O)([O-])[O-].[Na+].[Na+].O>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:13]([CH3:12])[CH2:14][CH2:15][NH:16][CH3:17])(=[O:10])=[O:9])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8070N,N'-DimethylethylenediamineHCID 95884-Fluorobenzenesulfonyl chlorideHCID 10340Sodium Carbonate

生成物 1

HCID 13712178HCID 13712178、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒4 回

実験手順

A solution of 4-fluorobenzenesulphonyl chloride (6.0 g) in chloroform (30 ml) was added dropwise to a well-stirred solution of N,N'-dimethyl-ethylenediamine (25 g) in chloroform (300 ml) at room temperature. After 2 hours the chloroform solution was vigorously shaken with aqueous sodium carbonate solution, separated, dried (MgSO4) and evaporated under reduced pressure to give an oil. The oil was treated with chloroform (60 ml) and water (100 ml). The two solvents were mixed thoroughly and were then separated. The chloroform layer was dried (MgSO4) and evaporated under reduced pressure to give an oil. Final traces of N,N'-dimethyl-ethylenediamine were removed by heating the oil under low vacuum to give 4-fluoro-N-methyl-N-[2-(methylamino)ethyl]benzenesulphonamide.

後処理

  1. customseparated
  2. dry with materialdried (MgSO4)
  3. customevaporated under reduced pressure
  4. customto give an oil
  5. additionThe two solvents were mixed thoroughly
  6. customwere then separated
  7. dry with materialThe chloroform layer was dried (MgSO4)
  8. customevaporated under reduced pressure
  9. customto give an oil
  10. customFinal traces of N,N'-dimethyl-ethylenediamine were removed
  11. temperatureby heating the oil under low vacuum

出典と根拠

ORDレコード
ord-462fd15b02c54a828f05357b256871a0
出典データセット
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04789677

反応ノート

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