反应详情

In 120 ml of dimethylformamide are dissolved 9.5 g (13 millimoles) of Z-Gln-Arg(Mts)-Leu-OH obtained according to the process of Example 20 and 5.2 g (16 millimoles) of Boc-Leu-OSu, and 1.43 ml of N-methylmorpholine is added to the solution. Then 0.5 g of 10% Pd-C is added to the mixture, and the mixture is stirred for 5 hours in a current of H2. The N-(2-aminoethyl)piperazine is added to the mixture, the mixture is stirred for 1 hour. The 10% Pd-C is recovered by filtration, and the mixture is cancentrated under reduced pressure. The residue is added to a liquid mixture of 100 ml of ethyl acetate and 200 ml of a dilute aqueous solution of citric acid. The mixture is sufficiently stirred, and the ethyl acetate layer is recovered, washed with water, dried and concentrated under reduced pressure. Ether is added to the concentrate and the precipitate is recovered by filtration to obtain 9.5 g of intended Boc-Leu-Gln-Arg(Mts)-Leu-OH (the yield being 86.5%).

1. customobtained
2. additionis added to the solution
3. stirringthe mixture is stirred for 1 hour
4. filtrationThe 10% Pd-C is recovered by filtration
5. additionThe residue is added to a liquid mixture of 100 ml of ethyl acetate and 200 ml of a dilute aqueous solution of citric acid
6. stirringThe mixture is sufficiently stirred
7. customthe ethyl acetate layer is recovered
8. washwashed with water
9. customdried
10. concentrationconcentrated under reduced pressure
11. additionEther is added to the
12. concentrationconcentrate
13. filtrationthe precipitate is recovered by filtration