[Cl:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]([NH2:12])=O)=[CH:8][CH:7]=1.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:24]2)=CC=1.O>C(Cl)(Cl)Cl.C1(C)C=CC=CC=1>[Cl:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:14]=[CH:13][C:9]([C:10](=[S:24])[NH2:12])=[CH:8][CH:7]=14-(3-Chloropropoxy)benzamide ax54 (1.0 g, 4.6 mmole, 1 eq) is dissolved in a 1:1 mixture of chloroform and toluene, 2,4-bis-(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (1.5 g, 3.7 mmole, 0.8 eq) is added. The reaction is stirred overnight at 85° C. Water is then added and the phases are separated. The organic layer is dried over magnesium sulfate and concentrated under reduce pressure. The crude material is purified by chromatography on silicagel (eluent: dichloromethane/methanol/ammonia 98:1.8:0.2) to provide 0.91 g of 4-(3-chloropropoxy)benzenecarbothioamide ax71 as a white solid.
Wird geladen…
