반응 #92032

반응 방정식

Cystamine dihydrochloride

DIEA

NHS-fluorescein

→

fluorescein cystamine

용매

DMF

ethyl acetate

반응 조건

후처리

1. 1
   기타the resulting reaction mixture
2. 2
   세척washed three times with water and one time with brine
3. 3
   건조The extract was dried over anhydrous sodium sulfate
4. 4
   농축concentrated under reduced pressure
5. 5
   workup.DISSOLUTIONredissolved in small amount of methanol and ethyl acetate
6. 6
   기타triturated with diethyl ether

실험 절차

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.

출처