Potassium nitrosodisulfonate → HCID 22506843、化合物

HRID 985571ノート

反応式

HRID 985571 の反応式
N(S([O-])(=O)=O)(S([O-])(=O)=[O:4])[O].[K+].[K+].[CH3:13][C:14]1([CH3:25])[CH2:22][C:21]2[C:16](=[C:17]([CH3:24])[CH:18]=[CH:19][C:20]=2[CH3:23])[NH:15]1>P([O-])([O-])([O-])=O.CO>[CH3:13][C:14]1([CH3:25])[CH2:22][C:21]2[C:16]([C:17]([CH3:24])=[CH:18][C:19](=[O:4])[C:20]=2[CH3:23])=[N:15]1

参加物

5

反応物 2

HCID 3032624Potassium nitrosodisulfonateHCID 22506883HCID 22506883、化合物

生成物 1

HCID 22506843HCID 22506843、化合物収率 72%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 1061Phosphate溶媒

実験手順

To a solution of 65% potassium nitrosodisulfonate (10.4 g, 25.2 mmol) in pH 6.86 phosphate buffer (320 ml) was added a solution of 2,3-dihydro-2,2,4,7-tetramethyl-1H-indole (2.21 g, 12.6 mmol) in methanol (50 ml) and stirred at room temperature for 1.5 hours. The reaction mixture was extracted three times with toluene. The organic layers were combined, washed with water and saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was subjected to a column chromatography on a silica gel (hexane:ethyl acetate=5:1) and recrystallized from ethyl acetate-hexane to obtain 1.71 g of the title compound.

後処理

  1. extractionThe reaction mixture was extracted three times with toluene
  2. washwashed with water and saturated brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customrecrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-966f2ea89d5f40ecbcad78287c321149
出典データセット
uspto-grants-2005_03
特許番号
US06872718B1

反応ノート

読み込み中…