反応 #792177

反応方程式

2-amino-3-methyl-5-chlorobenzoic acid

2-Amino-3-methyl-5-chlorobenzoic acid

product

2-Amino-3-methyl-5-chlorobenzoic acid

trichloromethyl chloroformate

→

title compound

6-Chloro-8-methyl-2H-3,1-benzoxazine-2,4(1H)-dione

溶媒

dioxane

反応条件

後処理

1. 1
   workup.DISSOLUTIONthe solid almost completely dissolved before a thick suspension
2. 2
   その他formed again

実験手順

To a suspension of 2-amino-3-methyl-5-chlorobenzoic acid (i.e. product of Example 6, Step A) (97 g, 520 mmol) stirred in dry dioxane (750 mL) at room temperature, trichloromethyl chloroformate (63 g, 320 mmol) was added dropwise. The reaction mixture exothermically warmed slowly to 42° C., and the solid almost completely dissolved before a thick suspension formed again. After the suspension was stirred at ambient temperature for 2.5 hours, the title compound was isolated by filtration, washed with ethyl ether, and dried to yield the title product compound, obtained as a white solid (98 g).

出典