反应详情

1,2-Dihydro-2-diazo-1-oxo-naphthalene-5-sulfonyl chloride (2.2 grams) is dissolved in dioxane (16 mls.) and the potassium salt of 4-hydroxyphenylazide (1.6 grams) in a mixture of water (4 ml.) and dioxane (4 ml.) is added gradually over a period of 10 minutes with stirring. The mixture is then stirred at room temperature (22°C) for 30 minutes to complete the reaction and then diluted with water (60 ml.) containing 3N hydrochloric acid (8 ml.). An oil separates out which solidifies on standing. The product is then collected and dried (2.5 grams). It is dissolved in benzene treated with carbon and filtered. Addition of 60°-80° pet. ether to the filtrate yields Compound 1. (1.7 grams) m.p. 136°-7° with decomposition.

1. additionis added gradually over a period of 10 minutes
2. stirringThe mixture is then stirred at room temperature (22°C) for 30 minutes
3. customthe reaction
4. customThe product is then collected
5. customdried (2.5 grams)
6. dissolutionIt is dissolved in benzene
7. additiontreated with carbon
8. filtrationfiltered
9. additionAddition of 60°-80° pet. ether to the filtrate