反应详情

温度

40 °C

10.1 g (0.05 mol) of 4,4-dihydroxydiphenyl ether (result of calculation of dipole moment based on MOPAC-97=0.73 debye) and 47.0 g (0.175 mol) of 4-naphthoquinone diazide sulphonyl chloride were dissolved in 500 g of 1,4-dioxane under a current of dry nitrogen, and then warmed to 40° C. To this there was added, dropwise, 17.7 g (0.175 mol) of triethylamine mixed with 50 g of 1,4-dioxane, in such a way that the internal temperature of the system did not rise to more than 45° C. Following the dropwise addition, stirring was carried out for 2 hours at 40° C. The by-product triethylamine hydrochloride was filtered off and the filtrate poured into 3 litres of 1% hydrochloric acid, after which the precipitate which was deposited was collected by filtering. Washing was carried out twice with 10 litres of water, and drying performed for 20 hours in a vacuum dryer at 50° C. Naphthoquinone diazide compound (1) was obtained. (On average, 1.75 of the Q groups=4-naphthoquinone diazide sulphonyl groups and 0.25=hydrogen.)

1. additionTo this there was added
2. customdid not rise to more than 45° C
3. additionthe dropwise addition
4. filtrationThe by-product triethylamine hydrochloride was filtered off
5. additionthe filtrate poured into 3 litres of 1% hydrochloric acid
6. customafter which the precipitate which was deposited was collected
7. filtrationby filtering
8. washWashing
9. customdrying
10. waitperformed for 20 hours in a vacuum dryer at 50° C