反応 #56606

反応方程式

Methyl 3-(5-phenylsulfonylbenzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydro-cinnamate

1,2,2,6,6-pentamethyl-4-hydroxy-piperidine

dioctyltin oxide

→

title compound

収率 70.0%

1,2,2,6,6-Pentamethylpiperidin-4-yl 3-(5-Phenylsulfonylbenzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamate

収率 70.0%

反応条件

後処理

1. 1
   その他At the end of six hours, any remaining xylene is removed by distillation under vacuum
2. 2
   その他The crude yellow oil obtained
3. 3
   その他is chromatographed through a pad of silica gel

実験手順

Methyl 3-(5-phenylsulfonylbenzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydro-cinnamate (5 g, 0.01 mol), xylenes (18 g, 0.17 mol), 1,2,2,6,6-pentamethyl-4-hydroxy-piperidine (2.1 g, 0.012 mol) and dioctyltin oxide (0.5 g, 0.0014 mol) are charged to a reactor and heated to 160° C. while being vigorously stirred. At the end of six hours, any remaining xylene is removed by distillation under vacuum. The crude yellow oil obtained is chromatographed through a pad of silica gel using ethyl aetate as the eluent. The title compound is obtained in a 70% yield as a low melting yellow solid, melting at 45-52° C., whose structure is consistent with 1Hnmr and mass spectrometry.

出典