反応 #10409

反応方程式

2-Amino-4,5-difluorobenzoic acid, 2,2-dibenzylhydrazide

triphosgene

NaHCO3

→

title compound

収率 198.7%

3-Dibenzylamino-6,7-difluoro-1H-quinazoline-2,4-dione

収率 198.7%

溶媒

methylene chloride

反応条件

後処理

1. 1
   その他the layers are separated
2. 2
   洗浄the aqueous layer is washed three times with ethyl acetate
3. 3
   乾燥The combined organic layers are dried over magnesium sulfate
4. 4
   濃縮concentrated

実験手順

2-Amino-4,5-difluorobenzoic acid, 2,2-dibenzylhydrazide (Example 15) (0.81 g, 2.2 mmol) and triphosgene (0.33 g, 1.1 mmol) are combined in 100 mL of methylene chloride and stirred at 25° C. for 20 hours. The solution is poured into 200 mL of saturated NaHCO3, the layers are separated, and the aqueous layer is washed three times with ethyl acetate. The combined organic layers are dried over magnesium sulfate and then concentrated to give 0.86 g of the title compound as a solid. MS CI: m/z 394 (MH+).

出典