Phosphorus sulfide (P2S5) → HCID 178516002、化合物

反応式

[C:1]1([N:7]2[CH:12]=[CH:11][C:10]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][C:18]3[N:19]=[N:20][NH:21][CH:22]=3)=[C:9]([OH:23])[C:8]2=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:26].C1(N2C=CC(CCCC3N=NNC=3)=C(O)C2=S)C=CC=CC=1>>[C:1]1([N:7]2[CH:12]=[CH:11][C:10]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][C:18]3[N:19]=[N:20][NH:21][CH:22]=3)=[C:9]([OH:23])[C:8]2=[S:26])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

反応物 3

HCID 14817Phosphorus sulfide (P2S5)

HCID 178515982HCID 178515982、化合物

HCID 178516891HCID 178516891、化合物

生成物 1

HCID 178516002HCID 178516002、化合物収率 121.3%

実験手順

Reaction of 159d (0.025 g, 0.077 mmol) and P4S10 (0.020 g, 0.046 mmol) under neat conditions as described for synthesis of 162b gave compound 162d (0.019 g, 73%) as a olive green solid. 1H NMR (400 MHz, DMSO) δ 8.55 (d, J=2.9 Hz, 2H), 7.83 (t, J=7.8 Hz, 3H), 7.43 (q, J=7.4 Hz, 2H), 7.32 (t, J=6.6 Hz, 1H), 7.08 (m, 1H), 6.92 (dd, J=31.0, 6.8 Hz, 1H), 6.81 (m, 1H), 4.51 (m, 2H), 4.41 (t, J=7.0 Hz, 2H), 1.89 (m, 4H), 1.32 (m, 2H). 13C NMR (100 MHz, CDCl3) δ 168.37, 155.10, 147.66, 131.04, 130.46, 128.75, 128.05, 125.57, 119.68, 113.69, 111.96, 57.73, 49.73, 29.47, 27.12, 23.04. HRMS (EI) calcd for C18H20N4OS [M]+ 340.135. found 326.1364.