Реакция #92032

ord-ce9c8c2a793b4da39941669816888f57

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеthe resulting reaction mixture
  2. 2
    Промывкаwashed three times with water and one time with brine
  3. 3
    СушкаThe extract was dried over anhydrous sodium sulfate
  4. 4
    Концентрированиеconcentrated under reduced pressure
  5. 5
    workup.DISSOLUTIONredissolved in small amount of methanol and ethyl acetate
  6. 6
    Другоеtriturated with diethyl ether

Методика

Cystamine dihydrochloride (68 mg, 0.301 mmol) and DIEA (110 μL, 2.1 eq.) were dissolved in DMF (10 mL), followed by addition of NHS-fluorescein, a mixture of 5- and 6-carboxyfluorescein (300 mg, 0.634 mmol) and the resulting reaction mixture was stirred overnight at room temperature. Then it was diluted with ethyl acetate and washed three times with water and one time with brine. The extract was dried over anhydrous sodium sulfate, concentrated under reduced pressure, redissolved in small amount of methanol and ethyl acetate, and then triturated with diethyl ether to obtain 140 mg of fluorescein-cystamine adduct as a bright orange solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09447035B2uspto-grants-2016_09