반응 #10409

반응 방정식

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

triphosgene

NaHCO3

→

title compound

수율 198.7%

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

수율 198.7%

용매

methylene chloride

반응 조건

후처리

1. 1
   기타the layers are separated
2. 2
   세척the aqueous layer is washed three times with ethyl acetate
3. 3
   건조The combined organic layers are dried over magnesium sulfate
4. 4
   농축concentrated

실험 절차

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+).

출처