反应详情

温度

-25 °C

5.94 (8.55 mM) of Boc-Ile-Phe-Thr-Asn-Ser-NH-NH2 are dissolved in 27 ml of DMSO plus 37 ml of DMF. After cooling to -25° C., 6.1 ml of a 5.6N HCl/dioxane solution, then 1.23 ml of tertiobutyl nitrite (1.2 equiv.) prediluted in 5 ml of DMF precooled to -20° C., are added. After 1 hr. 15 mins. of stirring between -20° C. and -25° C., 6.1 ml of diisopropylethylamine (DIPEA) are added to take the pH to around 6, then 3 ml of DMF are added to take the volume to 85 ml and this solution is conserved at -25° C.

1. customprecooled to -20° C.
2. additionare added
3. custom15 mins
4. customis conserved at -25° C.