Yield:342613-14-3 81%

Reaction Conditions:

with acetic acid;zinc at 60 - 70; for 5 h;

Steps:

1

Pour 80 ml acetic acid and 12 g active zinc powder into a reaction container, stirring evenly, increase temperature to 60-70 degrees C, add 5 g of 2'-TBS-7,10-TROC- docetaxel, and stir for 5 hrs until TLC shows the reaction completion. After filtering, add 80 ml of ethyl acetate and 80 ml of water into the filter liquor, extract, wash the organic layer with 50 ml of water, saturated NaHC0₃ (50 ml x 2), saturated NaCI (50 ml). Then dry with anhydrous Na₂S0₄. Filter and then evaporate the solution to gain white solid 2'-TBS-Docetaxel 2.5 g (yield 81 %). [0122] MS(m/z) :972(M+Na)? ,H MR (500MHz) δ 0.31 (6H, m),0.92 (9H, m),1.13(3H, s) , 1.30 (12H, m) , 1.72 (7H, m) , 1.92 (4H, m) , 2.18 (1H, m) , 2.35 (1H, m) , 2.61 (4H, m) , 3.95 (1H, d) ,4.21(3H,m) ,4.28 (1H, d) ,4.54(1H,s),4.97(lH,d) ,5.21 (lH.s) ,5.27(lH,m) ,5.50 (1H, m) ,5.70 (1H, d) ,6.31 (1H, t) ,7.29(2H,m) ,7.37 (2H, t) ,7.59 (1H, t) ,8.11 (1H, d) ,

References:

WO2013/57260,2013,A1 Location in patent:Page/Page column 34