反应详情

温度

0 °C

To 40 ml of mixed solvent of anhydrous methanolmethylene chloride was dissolved 0.5 g/0.8 mmol of 1,10-bis(3',5'-dimethyl-4'-acetoxyphenylcarbonyl)-1,10-diaza-4,7,13,16-tetraoxacyclooctadecane, and the solution was cooled to 0° C. To this solution was added 2.6 ml of freshly prepared 1M methanol solution of sodium methoxide, and the mixture was stirred at 0° C. for 2 hours. After adding Amberlite 15 until the reaction solution became neutral, the resin was separated by filtration and the filtrate was concentrated under reduced pressure to obtain 0.4 g of 1,10-bis(3',5'-dimethyl-4'-hydroxyphenylcarbonyl)-1,10-diaza-4,7,13,16-tetraoxacyclooctadecane. 1H-NMR (CDCl3): δ2.15 (12H, s), 3.6 (16H, br), 3.8 (8H, br), 5.89 (2H, s), 6.90 (4H, s).

1. additionAfter adding Amberlite 15 until the reaction solution
2. customthe resin was separated by filtration
3. concentrationthe filtrate was concentrated under reduced pressure