反应详情

温度

42.5 °C

A solution of 36.0 g (116 mmol) of 4-n-butylamino-1-cyclohexyloxy-2,2,6,6-tetramethylpiperidine in 100 ml of xylene is added over 20 minutes to a mixture of 10.9 g (59.2 mmol) of cyanuric chloride, 10.0 g of 50% aqueous sodium hydroxide, 10 ml of water, and 50 ml of xylene. The reaction temperature increases from 25 to 60° C. during the addition and is then maintained at 65°-70° C. for six hours. The phases are separated, and the organic phase is dried over magnesium sulfate and concentrated. The residue is purified by flash chromatography (39:1 heptane:ethyl acetate) on silica gel to afford 27.7 g (65% yield) of 2-chloro-4,6-bis-[N-(1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl)-n-butylamino]-1,3,5-triazine, a white glass, m.p. 75°-82° C.

1. temperatureis then maintained at 65°-70° C. for six hours
2. customThe phases are separated
3. dry with materialthe organic phase is dried over magnesium sulfate
4. concentrationconcentrated
5. customThe residue is purified by flash chromatography (39:1 heptane:ethyl acetate) on silica gel