Potassium nitrosodisulfonate → HCID 22506843, 화합물

HRID 985571노트

반응식

HRID 985571 반응식
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

참가 물질

5

반응물 2

HCID 3032624Potassium nitrosodisulfonateHCID 22506883HCID 22506883, 화합물

생성물 1

HCID 22506843HCID 22506843, 화합물수율 72%

시약·촉매·용매 2

HCID 887Methanol용매HCID 1061Phosphate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-966f2ea89d5f40ecbcad78287c321149
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06872718B1

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