반응 #420298

반응 방정식

tricarbonyl rhenium(I) 6-(bis(pyridin-2-ylmethyl)amino)hexylamine trifluoroacetate

4-isothiocyanatobenzenesulfonamide

triethylamine

→

solid

수율 96.0%

Tricarbonyl Rhenium(I) 4-(3-(8-(bis(pyridin-2-ylmethyl)amino)octyl)thioureido)-benzenesulfonamide

수율 96.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated
2. 2
   기타the resulting solid recrystallized from methanol/water

실험 절차

To a suspension of 4-isothiocyanatobenzenesulfonamide (11 mg, 0.05 mmol) in dry acetonitrile (1 mL) and triethylamine (15 μL, 0.11 mmol) was added tricarbonyl rhenium(I) 6-(bis(pyridin-2-ylmethyl)amino)hexylamine trifluoroacetate (40 mg, 0.48 mmol). The reaction mixture was stirred for 3 h at room temperature. The reaction mixture was concentrated and the resulting solid recrystallized from methanol/water to afford MIP-1140 as an off-white solid (38 mg, 96%). 1H NMR (400 MHz, DMSO-d6) δ 9.83 (br, 1H), 8.80 (d, J=5.4 Hz, 2H), 8.11 (br, 1H), 7.96 (m, 2H), 7.86-7.25 (m, 10H), 4.90 (m, 4H) 3.72 (m, 2H), 3.47 (br, 2H), 1.83 (br, 2H), 1.57 (m, 2H), 1.37 (bm, 8H); (M+H)+ (811).

출처