HRMS (ESI+): calcd for C12H10N3OS: 244.0545; discovered: 244.0542. (8d): Dihydrokaempferol Reaction period: 45 min; Produce: 97%; 148 mg; white solid; R9.20 (1H, s, H2), 8.46 (1H, d, = 8.8 Hz, H4), 8.31 (1H, s, H7), 7.86 (1H, d, = 8.8 Hz, H5), 5.21C5.06 (1H, m, NCH), 2.71C2.55 (2H, m, CH2), 2.54C2.35 (2H, m, CH2), 2.05C1.90 (2H, m, CH2); 13C-NMR (CDCl3, 25 C, 75.4 MHz): 159.0 (C), 157.8 (CH), 152.6 (C), 146.8 (C), 143.8 (CH), 130.5 (C), 129.5 (CH), 126.1 (CH), 116.3 (C), 50.9 (CH), 29.9 (2 CH2), 15.5 (CH2). spectra (ESI, EI, Rabbit polyclonal to Amyloid beta A4 and field desorption (FD)) had been documented with an LCP 1er XR spectrometer (WATERS, Guyancourt, France). Microwave-assisted reactions had been completed in sealed pipes having a Biotage Initiator microwave synthesis device, and temperatures had been assessed by IR-sensor (Biotage, Uppsala, Sweden). Period indicated in the many protocols may be the ideal period measured once the mixtures were in the programmed temp. The purity of most tested substances was dependant on chromatographic evaluation performed at 25 C on Best 3000 (Thermo Scientific, Les Ulis, France) having a quaternary pump built with a photodiode array detector (Father) handled at 254 nm. Column was a Luna C18 (150 mm 4.6 mm; 3 m particle size) supplied by Phenomenex (Le Pecq, France). The cellular phase was drinking water (A) and acetonitrile (B) ((8a): Response period: 55 min; Dihydrokaempferol Produce: 98%; 112 mg; white solid; R9.22 (1H, s, H2), 8.48 (1H, d, = 8.8 Hz, H4), 8.20 (1H, s, H7), 7.87 (1H, d, = 8.8 Hz, H5), 3.73 (3H, s, CH3); 13C1H-NMR (CDCl3, 25 C, 75.4 MHz): 160.2 (C), 157.8 (CH), 152.5 (C), 147.1 (C), 146.5 (CH), 130.2 (C), 129.3 (CH), 126.1 (CH), 116.3 (C), 34.3 (CH3). HRMS (ESI+): Calcd for C10H7N3OS [M + H]+: 218.0388; Found out: 218.03386. (8b): Response period: 45 min; Produce: 99%; 145 mg; beige solid; R9.19 (1H, s, H2), 8.44 (1H, d, = 8.8 Hz, H4), 8.25 (1H, s, H7), 7.84 (1H, d, = 8.8 Hz, H5), 5.37C5.12 (1H, m, NCH), 1.55 (3H, s, CH3), 1.53 (3H, s, CH3); 13C1H-NMR (CDCl3, 25 C, 75.4 MHz): 159.6 (C), 157.7 (CH), 152.5 (C), 146.6 (C), 143.4 (CH), 130.6 (C), 129.4 (CH), 126.0 (CH), 116.4 (C), 47.0 (CH), 22.2(2 CH3). HRMS (ESI+): Calcd for C12H11N3OS [M + H]+: 246.0701; Found out: 246.0708. (8c), was referred to in ref [15], normal data: 1H-NMR (CDCl3, 300 MHz): = 9.22 (s, 1H, H2), 8.49 (d, = 8.7 Hz, 1H, H4), 8.26 (s, 1H, H7), 7.87 (d, = 8.7 Hz, 1H, H5), 3.50C3.25 (m, 1H, NCH), 1.37C1.17 (m, 2H, CH), 1.12C0.91 (m, 2H, CH). HRMS (ESI+): calcd for C12H10N3OS: 244.0545; discovered: 244.0542. (8d): Response period: 45 min; Produce: 97%; 148 mg; white solid; R9.20 (1H, s, H2), 8.46 (1H, d, = 8.8 Hz, H4), 8.31 (1H, s, H7), 7.86 (1H, d, = 8.8 Hz, H5), 5.21C5.06 (1H, m, NCH), 2.71C2.55 (2H, m, CH2), 2.54C2.35 (2H, m, CH2), 2.05C1.90 (2H, m, CH2); 13C-NMR (CDCl3, 25 C, 75.4 MHz): 159.0 (C), 157.8 (CH), 152.6 (C), 146.8 (C), 143.8 (CH), 130.5 (C), 129.5 (CH), 126.1 (CH), 116.3 (C), 50.9 (CH), 29.9 (2 CH2), 15.5 (CH2). HRMS (ESI+): Calcd for C13H11N3OS [M + H]+: Dihydrokaempferol 258.0701; Found out: 258.0701. (8e): Response period: 45 min; Produce: 98%; 160 mg; white solid; R9.22 (1H, s, H2), 8.49 (1H, d, = 8.8 Hz, H4), 8.27 (1H, s, H7), 7.87 (1H, d, = 8.8 Hz, H5), 5.36C5.20 (1H, m, NCH), 2.38C2.21 (2H, m, CH2), 2.12C1.74 (2H, m, CH2); 13C1H-NMR (CDCl3, 25 C, 75.4 MHz): 159.8 (C), 157.7 (CH), 152.3 (C), 146.4 (C), 144.1 (CH), 130.4 (C), 129.2 (CH), 125.8 (CH), 116.1 (C), 56.4 (CH), 32.1 (2 CH2), 24.5 (2 CH2). HRMS (ESI+): Calcd for C14H13N3OS [M + H]+: 272.0858; Found out: 272.0855. (8f): Response period: 90 min; Produce: 98%;.
HRMS (ESI+): calcd for C12H10N3OS: 244