反应详情

温度

-10 °C

2.1 ml N-methylmorpholine are added with stirring to a solution of 6.3 g Boc-Cys(MBzl)-OH in 50 ml THF, followed by drop-wise addition at -15° C. of 2.4 ml chloroformic acid isobutyl ester. After stirring for 5 minutes at -15° C. a solution of 3.3 g H-Thr-ol hydrochloride and 4.1 ml N-methylmorpholine in 30 ml DMF, pre-cooled to -10° C. is added. The reaction mixture is stirred for 2 hrs. at 0° C. and for a further 2 hrs. at room-temperature. 50 ml 10% KHCO3 -solution are added and the whole concentrated under vacuum. After dilution with AcOEt, washing 3× with 2 N citric acid, 3× with KHCO3 -solution and 1× with NaCl solution, the organic phase is dried over Na2SO4 and evaporated under vacuum to yield the title compound:

1. additionis added
2. waitat 0° C. and for a further 2 hrs
3. concentrationthe whole concentrated under vacuum
4. washAfter dilution with AcOEt, washing 3× with 2 N citric acid, 3× with KHCO3 -solution and 1× with NaCl solution
5. dry with materialthe organic phase is dried over Na2SO4
6. customevaporated under vacuum