反应详情

5.0 g. of methoxy amine was dissolved in 100 ml. of H2O. Then, 14.0 g. of 2,4,5-trichlorobenzene sulfonyl chloride dissolved in 25 ml. of tetrahydrofuran was added under high speed mechanical stirring. Then, 8.8 g. of sodium hydroxide in a 50% solution + 10 ml. of water was dropped in at room temperature. An exothermic reaction took place and the temperature went up to 37.5° C. When the reaction subsided, it was stirred at room temperature for two hours and the solid was then filtered off and stirred into 150 ml. of ether for 1 hour. The solid was removed by filtration to yield 11.3 g. of product. The product was redissolved in ether. The ether was evaporated to yield 7.4 g. of product, m.p. 163°-166° C.

1. customAn exothermic reaction
2. customwent up to 37.5° C
3. filtrationthe solid was then filtered off
4. stirringstirred into 150 ml
5. waitof ether for 1 hour
6. customThe solid was removed by filtration
7. customto yield 11.3 g
8. customThe ether was evaporated
9. customto yield 7.4 g