反应详情

温度

50 °C

A mixture of 4-(2-nitro-4,5-dimethylphenoxymethyl)-3-methylbenzoic acid methyl ester prepared in Reference Example 1 (7.21 g), acetic acid (88 ml) and water (8.8 ml) was stirred at 50° C. To the reaction solution, iron powder (6.11 g) was gradually added, and the mixture was stirred for 1 hour at 50° C. After cooling, the mixture was filtered and the filtrate was concentrated and azeotroped with toluene. To the residue, ethyl acetate-water (100 ml-100 ml) was added and the mixture was filtrated over Celite (registered trademark). The organic layer was washed, dried, concentrated under reduced pressure to give the title compound (4.66 g) having the following physical data.

1. stirringthe mixture was stirred for 1 hour at 50° C
2. temperatureAfter cooling
3. filtrationthe mixture was filtered
4. concentrationthe filtrate was concentrated
5. customazeotroped with toluene
6. additionTo the residue, ethyl acetate-water (100 ml-100 ml) was added
7. filtrationthe mixture was filtrated over Celite (registered trademark)
8. washThe organic layer was washed
9. customdried
10. concentrationconcentrated under reduced pressure