反应详情

温度

25 °C

250 mg of Z-Sta-OH(cf. stage 1.12) are dissolved in 4 ml of 90% strength methanol. 1 ml of a 20% aqueous cesium carbonate solution is added to the solution, and the solvent is then removed in a rotary evaporator. The residue is twice dissolved in 2.5 ml of DMF and each time the DMF is removed again in a rotary evaporator. The residue is dried in a high vacuum, then dissolved in 2.5 ml of DMF and 55 μl of methyl iodide are added to the solution. The whole is stirred for 18 hours at 25° C., the solvent is then removed and the residue is taken up in ethyl acetate. After extraction twice with sodium chloride solution, the organic phase is dried over sodium sulphate and concentrated by evaporation. The residue is flash-chromatographed over 55 g of silica gel (eluant: chloroform/methanol [95:5]). The product-containing fractions are combined and concentrated by evaporation, yielding Z-Sta-OMe in the form of a yellowish oil; Rf (chloroform/methanol [95:5])=0.49.

1. customthe solvent is then removed in a rotary evaporator
2. dissolutionThe residue is twice dissolved in 2.5 ml of DMF
3. customeach time the DMF is removed again in a rotary evaporator
4. customThe residue is dried in a high vacuum
5. dissolutiondissolved in 2.5 ml of DMF
6. addition55 μl of methyl iodide are added to the solution
7. customthe solvent is then removed
8. extractionAfter extraction twice with sodium chloride solution
9. dry with materialthe organic phase is dried over sodium sulphate
10. concentrationconcentrated by evaporation
11. customThe residue is flash-chromatographed over 55 g of silica gel (eluant: chloroform/methanol [95:5])
12. concentrationconcentrated by evaporation