反应详情

To stirring suspension of 4-(heptyloxy)benzamide (1.24 g, 5.29 mmol) in DME (20 mL) and THF (10 mL) was added 2,4-bis(4-phenoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (2.80 g, 5.29 mmol). The reaction mixture was stirred at RT for 16 h. The reaction mixture was concentrated onto silica and purified by column chromatography (0-60% EA in iso-hexanes) to afford 1.4 g (62%) of 4-(heptyloxy)benzothioamide as a yellow waxy solid. LCMS-ESI (m/z) calculated for C14H21NOS: 251.4. found 252.0 [M+H]+, tR=3.13 min. (Method 6).

1. stirringThe reaction mixture was stirred at RT for 16 h
2. concentrationThe reaction mixture was concentrated onto silica
3. custompurified by column chromatography (0-60% EA in iso-hexanes)