o-Toluenesulfonyl chloride → HCID 22099729、化合物

HRID 1457647ノート

反応式

HRID 1457647 の反応式
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][CH2:6][CH2:7][NH:8][C:9]1[CH:18]=[CH:17][CH:16]=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[CH3:2].[CH3:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[S:27](Cl)(=[O:29])=[O:28]>N1C=CC=CC=1>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][CH2:6][CH2:7][N:8]([C:9]1[CH:18]=[CH:17][CH:16]=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[S:27]([C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[CH3:20])(=[O:29])=[O:28])[CH3:2]

参加物

4

反応物 2

HCID 8623o-Toluenesulfonyl chlorideHCID 266836Methyl 2-[(4-ethoxy-4-oxobutyl)amino]benzoate

生成物 1

HCID 22099729HCID 22099729、化合物収率 90.7%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 2.65 g of methyl 2-[(4-ethoxy-4-oxobutyl)amino]benzoate, 2.0 g of 2-methylphenylsulfonyl chloride and pyridine is heated on a steam bath for 16 hours. The mixture is concentrated under a vacuum (remove pyridine) and 1N HCl added. The mixture is extracted with dichloromethane and the extract washed with 1NHCl, H2O, 1M NaHCO3, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrons magnesium silicate and the filtrate evaporated to give 3.8 g of solid which is crystallized from ethanol to give crystals, m.p. 100°-102° C.

後処理

  1. temperatureis heated on a steam bath for 16 hours
  2. concentrationThe mixture is concentrated under a vacuum (remove pyridine) and 1N HCl
  3. additionadded
  4. extractionThe mixture is extracted with dichloromethane
  5. washthe extract washed with 1NHCl, H2O, 1M NaHCO3, brine
  6. dry with materialdried (Na2SO4)
  7. filtrationThe solution is filtered through a thin pad of hydrons magnesium silicate
  8. customthe filtrate evaporated

出典と根拠

ORDレコード
ord-8fef0a5ed1474e2fb06b85677cec9daf
出典データセット
uspto-grants-1998_12
特許番号
US05849735

反応ノート

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