Phosphorus sulfide (P2S5) → HCID 178515998、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][C:17]3[N:18]=[N:19][NH:20][CH:21]=3)=[C:9]([OH:22])[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:25].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][C:17]3[N:18]=[N:19][NH:20][CH:21]=3)=[C:9]([OH:22])[C:8]2=[S:25])[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 178516890HCID 178516890、化合物

生成物 1

HCID 178515998HCID 178515998、化合物収率 85.2%

実験手順

Reaction of 159c (0.055 g, 0.18 mmol) and P4S10 (0.051 g, 0.115 mmol) under neat conditions as described for synthesis of 162b gave compound 162c (0.032 g, 55%) as a olive green solid. δ 8.50 (s, 1H), 7.81 (m, 3H), 7.36 (m, 4H), 6.94 (d, J=7.6 Hz, 1H), 6.62 (t, J=6.8 Hz, 1H), 4.54 (t, J=7.6 Hz, 2H), 4.46 (t, J=6.4 Hz, 2H), 2.03 (m, 4H). 13C NMR (100 MHz, CDCl3) δ 168.51, 155.08, 147.73, 131.02, 130.36, 128.79, 128.13, 125.58, 119.91, 113.87, 112.10, 56.96, 49.41, 27.02, 25.08. HRMS (EI) calcd for C17H18N4OS [M]+ 326.1201. found 326.1200.