반응 #62962

반응 방정식

neocarzinostatin

NCS

trinitrobenzene sulfonic acid

→

nitrobenzene

용매

—

aqueous solution

sodium bicarbonate

반응 조건

후처리

1. 1
   온도cooling in the dark
2. 2
   workup.ADDITIONThe powdery H-SMA stepwise was added in a total amount of 0.5 g in several times
3. 3
   workup.DISSOLUTIONdissolved
4. 4
   기타During the reaction
5. 5
   기타taken out from the reaction mixture 24 hours
6. 6
   workup.ADDITIONafter the addition
7. 7
   workup.ADDITIONwas started was diluted

실험 절차

20 g of neocarzinostatin (NCS) was dissolved in 5.0 ml of 0.8M aqueous solution of sodium bicarbonate under ice-cooling in the dark. The powdery H-SMA stepwise was added in a total amount of 0.5 g in several times and dissolved thereinto. During the reaction,, the pH of the solution was kept around 8.5. The conversion of such an unreacted primary amino group originating from NCS can be determined by a method (hereinafter referred to as "TNBS" method) in which a small amount of a sample taken out from the reaction mixture 24 hours after the addition was started was diluted, and was reacted with trinitrobenzene sulfonic acid to produce a nitrobenzene derivative, which was determined based on the amount of the primary amino group spectrophotometrically by a visible absorption spectrometer at 420 nm. It was learned that the primary amino groups completely disappeared.

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