反応 #43266

反応方程式

ethyl 2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-3-(tetrahydropyran-4-yl)propionate

NaOH

→

2-(10-Methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-3-(tetrahydropyran-4-yl)propionic Acid

溶媒

methanol

反応条件

後処理

1. 1
   その他The methanol is removed under reduced pressure
2. 2
   workup.ADDITIONthe reaction mixture is adjusted to pH 4 by addition of concentrated hydrochloric acid
3. 3
   抽出The mixture is extracted three times with in each case 100 ml of ethyl acetate
4. 4
   乾燥The combined organic phases are dried over MgSO4
5. 5
   濃縮concentrated under reduced pressure

実験手順

2.0 g of ethyl 2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-3-(tetrahydropyran-4-yl)propionate are suspended in 100 ml of methanol, and 32.1 ml of a 2M NaOH solution are added. The reaction mixture is stirred at 80° C. for one hour. The methanol is removed under reduced pressure and the reaction mixture is adjusted to pH 4 by addition of concentrated hydrochloric acid. The mixture is extracted three times with in each case 100 ml of ethyl acetate. The combined organic phases are dried over MgSO4 and then concentrated under reduced pressure. This gives 1.85 g of 2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-3-(tetrahydropyran-4-yl)propionic acid as a solid.

出典