反応 #6456

反応方程式

5,5-dimethyl-1,3-cyclohexanedione

triethylamine

benzothiadiazole-7-carboxylic acid chloride

→

title compound

収率 87.5%

3-(benzo-1,2,3-thiadiazole-7-carbonyloxy)-5,5-dimethyl-cyclohex-2-enone

収率 87.5%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   洗浄The ethyl acetate solution is washed with H2O
2. 2
   その他dried
3. 3
   濃縮concentrated
4. 4
   その他Purification by column chromatography

実験手順

5.6 g (0.04 mol) of 5,5-dimethyl-1,3-cyclohexanedione are dissolved in a mixture of 4.4 g (0.044 mol) of triethylamine and 120 ml of ethyl acetate. 8.7 g (0.044 mol) of benzothiadiazole-7-carboxylic acid chloride are added dropwise at 15° to 20° C., and the mixture is subsequently stirred overnight at room temperature. The ethyl acetate solution is washed with H2O, dried and concentrated. Purification by column chromatography using ethyl acetate/hexane gives 10.5 g (87.5%) of the title compound, melting point 131°-133° C.

出典