反応 #433765

反応方程式

Trichloromethyl chloroformate

Compound 10

2-Amino-5-methyl benzoic acid

→

white solids

収率 94.1%

6-Methyl-1H-benzo[d][1,3]oxazine-2,4-dione

収率 94.1%

溶媒

dioxane

反応条件

後処理

1. 1
   温度the solution was refluxed for 4 h
2. 2
   温度The solution was cooled in ice bath
3. 3
   その他the solids formed
4. 4
   ろ過were filtered
5. 5
   洗浄The solids were washed by ether
6. 6
   その他dried under vacuum at room temperature

実験手順

Trichloromethyl chloroformate (36.27 mL, 300 mmol) was added to a stirred solution of Compound 10 (41.3 g, 273 mmol) in dry dioxane at room temperature and the solution was refluxed for 4 h. The solution was cooled in ice bath and the solids formed were filtered. The solids were washed by ether and dried under vacuum at room temperature to yield 45.5 g (94%) of white solids. M.P. 257° C. 1H NMR (DMSO-d6): δ 2.32 (s, 3H), 7.06 (d, J=8.6 Hz, 1H), 7.56 (dd, J=8.6, 1.8 Hz, 1H), 7.71 (d, J=1.1, 1H), 11.63 (s, 1H). EIMS (neg. mode) m/z 176 (M−1), 152 (M+23). Anal. (C9H7NO3) C, H, N.

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