反応 #155328

反応方程式

sodium hydroxide

ethyl[3-(4-methoxyphenyl)-4-oxo-10-propoxy-7,8-dihydro-4H,6H-5-oxa-1-aza-phenanthren-1-yl]acetate

→

[3-(4-methoxyphenyl)-4-oxo-10-propoxy-7,8-dihydro-4H,6H-5-oxa-1-aza-phenanthren-1-yl]acetic acid

収率 88.4%

溶媒

ethanol

反応条件

後処理

1. 1
   温度heated for 2 hours
2. 2
   温度under reflux
3. 3
   濃縮concentrated under reduced pressure
4. 4
   温度While ice-cooling the concentrate, water and concentrated hydrochloric acid
5. 5
   workup.ADDITIONwere added to the residue
6. 6
   その他Subsequently, the formed insoluble matter was separated
7. 7
   その他dried

実験手順

A 5N aqueous sodium hydroxide solution (10 ml) was added to an ethanol solution (30 ml) of ethyl[3-(4-methoxyphenyl)-4-oxo-10-propoxy-7,8-dihydro-4H,6H-5-oxa-1-aza-phenanthren-1-yl]acetate (700 mg, 1.55 mmol) and heated for 2 hours under reflux. The mixture was cooled to room temperature and concentrated under reduced pressure. While ice-cooling the concentrate, water and concentrated hydrochloric acid were added to the residue to make it acidic. Subsequently, the formed insoluble matter was separated and dried, giving a yellow powder of [3-(4-methoxyphenyl)-4-oxo-10-propoxy-7,8-dihydro-4H,6H-5-oxa-1-aza-phenanthren-1-yl]acetic acid (580 mg, yield: 88%).

出典