Potassium Iodide → HCID 515415、化合物

反応式

Cl[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[S:18][C:17]3[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26]Cl)=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1)=[O:7].[I-].[K+].[CH2:31]([NH:34][CH2:35][CH:36]=[CH2:37])[CH:32]=[CH2:33]>O1CCCC1>[CH2:31]([N:34]([CH2:35][CH:36]=[CH2:37])[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[S:18][C:17]3[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26][N:34]([CH2:35][CH:36]=[CH2:37])[CH2:31][CH:32]=[CH2:33])=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1)=[O:7])[CH:32]=[CH2:33]

参加物

反応条件

温度: 120 °C

実験手順

A mixture of 22.3 g (0.05 mole) of 2,7-bis(5-chlorovaleryl)thioxanthene, 1 g of potassium iodide, 100 ml of diallylamine and 200 ml of tetrahydrofuran was placed in a Paar bomb and heated to 120°C. with stirring for 24 hours. Upon cooling, the mixture was filtered and the filtrate evaporated to dryness. The resulting residue was dissolved in dilute HCl and extracted with ether. The aqueous portion was made basic, extracted with methylene chloride, dried over magnesium sulfate and filtered. The filtrate was heated to boiling, treated with charcoal, filtered and filtrate evaporated to dryness. The residue was chromatographed on a column of alumina and eluted with methylene chloride. The resulting oil was dissolved in diethyl ether, dried over molecular sieves, filtered and the ether evaporated. This process was repeated several times to yield the desired product.