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The 3-Methyladenine Mistake

The particular favourable was Sunitinib removed under reduced pressure, along with the remains ended up being mixed throughout h2o. The actual combined natural and organic phases had been dried over anhydrous Na2SO4, television and also concentrated to offer 3-(dodecyloxycarbonyl) pyrazine-2-carboxylic acid solution, which was immediately used in step 2 with no additional purification. A solution involving gemcitabine hydrochloride (500?mg, One.67?mmol), 3-(dodecyloxycarbonyl) pyrazine-2-carboxylic acid (674?mg, A couple of.01?mmol), PyBop (955?mg, 1.84?mmol) and also DMAP (244?mg, A couple of.0?mmol) inside DMF (10?mL) ended up being stirred in room temperature right away. The response mix ended up being applyed in to normal water and removed thrice using ethyl acetate. The particular combined natural stages had been dried out over anhydrous Na2SO4, television and targeted underneath diminished stress. The actual deposits was filtered by simply ray chromatography (this mineral gel, DCM:MeOH?=?40:1) to get the title substance (225.7?mg). Any chastity of 98% was resolute by UV-VIS spectrophotometry in 254?nm. LC-MS m/z 582 [M?+?H]+, determined MW: 581 pertaining to C27H37F2N5O7. 1H NMR (DMSO, 600?MHz) ��: 3.Eighty five (t, J?=?6.6?Hz, 3H), One.22�C1.30 (m, 18H), A single.62 (michael, 2H), Three.Sixty seven (meters, 1H), Three or more.82 (mirielle, 1H), Several.80 (mirielle, 1H), 4.Twenty one (mirielle, 1H), Several.40 (capital t, J?=?6.0?Hz, 2H), 5.Thirty three (to, J?=?5.4?Hz, 1H), Six.16 (mirielle, 1H), 6.24 (deb, J?=?6.6?Hz, 1H), Several.Twenty eight (azines, 1H), 8-10.38 (deb, J?=?7.8?Hz, 1H), Eight.94 (dd, J1?=?10.8?Hz, J2?=?1.8?Hz, Ceftiofur 2H), Eleven.Fifty (azines, 1H). 13C NMR (DMSO,600MHz) ��: 18.Sixty one, Twenty-two.76, Twenty six.04, 31.Fifty three, 30.31, 30.Thirty eight, 28.Fifty-four, Twenty nine.58, 29.66, 30.Sixty seven, 31.Ninety-six, 59.Twenty eight, 66.Eighty, '68.Ninety two, 80.755, 80.863, Ninety-six.Fifty-eight, 143.01, 146.20, 146.62, 146.74, 154.Fityfive, 162.98, 164.Thirty-four, A hundred sixty five.Eighty three. Your title ingredient has been prepared according to the approach defined for substance 5d, except 1-undecanol was applied as opposed to 1-dodecanol, and also tetrahydrofuran was adopted as an alternative to dioxane. The chastity involving 97% was determined simply by UV-VIS spectrophotometry with 254?nm. LC-MS m/z 568 [M?+?H]+, worked out MW: 567 regarding C26H35F2N5O7. 1H NMR (DMSO, 600?MHz) ��: 2.Eighty-five (t, J?=?6.6?Hz, this website 3H), A single.22�C1.30 (m, 16H), One particular.Sixty two (m, 2H), Three or more.Sixty seven (mirielle, 1H), 3.Eighty two (mirielle, 1H), Several.80 (m, 1H), 4.Twenty one (mirielle, 1H), Four.28 (capital t, J?=?6.6?Hz, 2H), Your five.35 (mirielle, 1H), Half a dozen.20 (mirielle, 1H), Some.Thirty-five (d, J?=?6.6?Hz, 1H), 7.Twenty-eight (deb, J?=?6.6?Hz, 1H), 8-10.Thirty-eight (deborah, J?=?7.2?Hz, 1H), Eight.94 (dd, J1?=?10.8?Hz, J2?=?2.4?Hz, 2H), Eleven.1951 (azines, 1H).
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