反应详情

温度

95 °C

46.2 g of iron filings, 46 ml of water and 9 ml of glacial acetic acid are stirred for 30 minutes at 95° C. Then 150 ml of cyclohexanone are added and, when the temperature has again risen to 95° C., 36.8 g of (p-nitrophenoxy)methyl-1,4-dioxane (known from British patent specification 749 713) are added in portions. The batch is then stirred for 31/2 hours at 95° C. and, after addition of 9.0 g of sodium carbonate in portions, filtered hot. The residue is washed with cyclohexanone and the filtrate is subjected to steam distillation. After cooling, the product precipitates in the form of white crystals which are separated from a dark oil and recrystallised from water with the addition of animal charcoal. The crystals are dried in vacuo at 60° C., affording 16.3 g (51% of theory) of (p-aminophenoxy)methyl-1,4-dioxane of the formula ##STR33## with a melting point of 86°-87° C.

1. customhas again risen to 95° C.
2. filtrationfiltered hot
3. washThe residue is washed with cyclohexanone
4. distillationthe filtrate is subjected to steam distillation
5. temperatureAfter cooling
6. customthe product precipitates in the form of white crystals which
7. customare separated from a dark oil
8. customrecrystallised from water with the addition of animal charcoal
9. customThe crystals are dried in vacuo at 60° C.