反応 #721862

反応方程式

Acetic anhydride

4-(5-benzyloxy-2-fluoro-4-methylanilino)-7-(2-hydroxyethoxy)-6-methoxyquinazoline

triethylamine

water

→

7-(2-acetoxyethoxy)-4-(5-benzyloxy-2-fluoro-4-methylanilino)-6-methoxyquinazoline

収率 43.0%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   その他the organic layer separated
2. 2
   洗浄washed with water and brine
3. 3
   乾燥dried (MgSO4)
4. 4
   その他Most of the solvent was removed by evaporation and hexane
5. 5
   workup.ADDITIONadded
6. 6
   ろ過The precipitated product was collected by filtration

実験手順

Acetic anhydride (55 ml, 0.58 mmol) was added to a mixture of 4-(5-benzyloxy-2-fluoro-4-methylanilino)-7-(2-hydroxyethoxy)-6-methoxyquinazoline (233 mg, 0.52 mmol), triethylamine (80 ml, 0.57 mmol) and 4-(N,N-dimethylamino)pyridine (5 mg) in ethyl acetate (50 ml). The mixture was stirred for 2 hours at ambient temperature, water was added, the organic layer separated, washed with water and brine and dried (MgSO4). Most of the solvent was removed by evaporation and hexane added. The precipitated product was collected by filtration to give 7-(2-acetoxyethoxy)-4-(5-benzyloxy-2-fluoro-4-methylanilino)-6-methoxyquinazoline (110 mg, 43%).

出典