반응 #2074242

반응 방정식

2-{3-[2-(3-chlorophenyl)-2,2-difluoroethylamino]-6-cyano-2-fluorophenyl}-N-(2-amidinoaminooxyethyl)acetamide

HCl

HCl MeCN

→

title compound

수율 176.2%

N-[2-(Amidinoaminooxy)ethyl]-2-{3-[2-(3-chlorophenyl)-2,2-difluoroethylamino]-6-cyano-2-fluorophenyl}acetamide Hydrochloride

수율 176.2%

용매

MeCN

—

five

반응 조건

후처리

1. 1
   여과the resulting crystals were filtered
2. 2
   기타dried under vacuum

실험 절차

To a homogeneous pale yellow solution of 2-{3-[2-(3-chlorophenyl)-2,2-difluoroethylamino]-6-cyano-2-fluorophenyl}-N-(2-amidinoaminooxyethyl)acetamide (1.28 g, 2.74 mmol), as prepared in the preceding step, in dry MeCN (38 mL) was added anhydrous HCl (0.283 M in MeCN, 10.2 mL, 2.89 mmol) rapidly at room temperature in five ˜2 mL portions with swirling. Immediately following addition of the last portion of HCl/MeCN, the solution was allowed to sit undisturbed at room temperature for 15 min, and the resulting crystals were filtered and dried under vacuum to afford the title compound (1.22 g, 88%) as off-white microcrystals. 1H NMR (300 MHz, CD3OD) δ 7.57-7.54 (m, 1H), 7.52-7.41 (m, 3H), 7.29 (dd, J=8.6 Hz, 1.3 Hz, 1H), 6.80 (t, J=8.6 Hz, 1H), 3.95 (t, J=5.4 Hz, 2H), 3.94 (t, J=13.7 Hz, 2H), 3.76 (d, J=2.0 Hz, 2H), 3.52 (t, J=5.4 Hz, 2H). LC/MS (ESI) calcd for C20H21ClF3N6O2 (MH+) 469.1. found 469.1. Elem. Anal. Calc. for free base •1.00 HCl: C, 47.54; H, 4.19; N, 16.63; Cl, 7.02. Found: C, 47.42; H, 4.03; N, 16.62; Cl, 7.02. Karl Fischer % water: <0.10.

출처