Reaktion #792156

Reaktionsgleichung

2-amino-3-methylbenzoic acid

trichloromethyl chloroformate

→

off-white solid

8-Methyl-2H-3,1-benzoxazine-2,4(1H)-dione

Lösungsmittel

1,4-dioxane

1,4-dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe reaction temperature below 25° C
2. 2
   Sonstigeto form during the addition
3. 3
   SonstigeThe precipitated solids were removed by filtration
4. 4
   Waschenwashed with 1,4-dioxane (2×20 mL) and hexane (2×15 mL)
5. 5
   Sonstigeair-dried

Vorschrift

To a solution of 2-amino-3-methylbenzoic acid (6 g) in dry 1,4-dioxane (50 mL) was added dropwise a solution of trichloromethyl chloroformate (8 mL) in dry 1,4-dioxane (25 mL), with ice-water cooling to keep the reaction temperature below 25° C. A white precipitate began to form during the addition. The reaction mixture was stirred at room temperature overnight. The precipitated solids were removed by filtration and washed with 1,4-dioxane (2×20 mL) and hexane (2×15 mL) and air-dried to yield 6.51 g of off-white solid.

Quelle