반응 #1117642

반응 방정식

NAD+

thiophosgene

sodium carbonate

→

NAD NCS

용매

H2O

CHCl3

반응 조건

후처리

1. 1
   기타with attached bubble-counter
2. 2
   workup.ADDITIONa little Na2CO3 was added
3. 3
   workup.WAITAfter 3.5 hours there was no longer
4. 4
   기타The mixture was evaporated to dryness in vacuo
5. 5
   기타freeze-dried
6. 6
   기타The slightly brownish product mixture could be purified of by-products by column chromatography on silica gel
7. 7
   기타unpurified for the reaction with the polymer (see Example 2)
8. 8
   여과since purification by ultrafiltration of the product

실험 절차

2 mmol of NAD+ were dissolved in 10 ml of H2O in a round-bottomed flask with attached bubble-counter, and a little Na2CO3 was added. A solution of 20 mmol of thiophosgene in 10 ml of CHCl3 was added with vigorous stirring at 20° C. The pH was checked every 10 minutes and kept between 5.5 and 8.5 by the addition of small amounts of sodium carbonate. After 3.5 hours there was no longer any change in the pH, and no further gas was evolved. The mixture was evaporated to dryness in vacuo and freeze-dried. The slightly brownish product mixture could be purified of by-products by column chromatography on silica gel using water/acetonitrile as eluent. However, it is advisable to use the product mixture unpurified for the reaction with the polymer (see Example 2), since purification by ultrafiltration of the product immobilized on the polymer is considerably more straightforward and, moreover, the sensitivity of NAD-NCS results in losses due to dimerization and trimerization during purification.

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