反应详情

温度

50 °C

65.1 grams of the compound of Example 3 was added with stirring to a solution of 36 grams of sodium hydroxide in 40 ml of ethylene glycol and 66 ml of water. The reaction mixture became homogeneous at about 116° to 117° and was heated at this temperature for two hours. The reaction mixture was cooled by the addition of chopped ice and cold water to the reaction mixture to make a total volume of one liter. After clarifying the reaction mixture by filtration, the filtrate was made acid with concentrated aqueous hydrochloric acid, yielding a white precipitate, which was filtered, washed with cold water and dried. The product was then treated with rapid stirring at 50° C with about 800 ml of 6% sodium bicarbonate solution until carbon dioxide evolution stopped. The turbid solution was filtered free of a white solid-by-product. (A). The clarified filtrate was made acid with concentrated hydrochloric acid while cooling, and the resulting white precipitate filtered. After washing with hot water and drying the product was obtained as a white powder melting at 161° to 165°.

1. custombecame homogeneous at about 116° to 117°
2. temperaturewas heated at this temperature for two hours
3. filtrationby filtration
4. customyielding a white precipitate, which
5. filtrationwas filtered
6. washwashed with cold water
7. customdried
8. additionThe product was then treated
9. filtrationThe turbid solution was filtered free of a white solid-by-product
10. temperaturewhile cooling
11. filtrationthe resulting white precipitate filtered
12. washAfter washing with hot water
13. customdrying the product