反应详情

A 4-l. battery jar was charged charged with 641 g (4.23 moles) of 6-chloroindole, 926 g (5.3 moles) of crude (ca. 85% pure) alpha-nitro-beta-ethoxy acrylic acid methylester and 475 g (4.65 moles) of acetic anhydride. The mixture was well stirred at room temperature for 45 hours to give a highly viscous suspension of an orange precipitate. 1.5 l of a mixture of benzene-ether-hexane 1:1:3 was added and the mixture stirred vigorously for 30 minutes. The product was collected by filtration, washed with 1:0 l of the same solvent mixture and dried at room temperature and 16 mmHg to constant weight to afford 600 g (51%) of product as orange crystals, m.p. 159°-160°.

1. additionbattery jar was charged
2. customto give
3. additiona highly viscous suspension of an orange precipitate
4. stirringthe mixture stirred vigorously for 30 minutes
5. filtrationThe product was collected by filtration
6. washwashed with 1
7. dry with material0 l of the same solvent mixture and dried at room temperature