反应详情

Sodium nitrite, 5 g (0.072 mole), was added in portions over a period of 5 min to a solution of 20 g (0.06 mole) of 7-chloro-1,3-dihydro-5-(2-fluorophenyl)-2-nitromethylene-2H-1,4-benzodiazepine* in 100 ml of glacial acetic acid. Following the addition, the reaction mixture was stirred at room temperature for 15 min. The product, which crystallized partially during this period, was further precipitated by slow addition of 50 ml of water and collected by filtration. The crystals were washed with water, sucked dry and washed with methanol/ether to leave light yellow product. The filtrate was diluted with water and extracted with methylene chloride. The extracts were washed with water, dried and evaporated. Crystallization of the residue from methylene chloride/hexane yielded additional product. The analytical sample was recrystallized from ether to give pale yellow crystals with mp 220°-230° C. dec.

1. additionthe addition
2. customThe product, which crystallized partially during this period
3. customwas further precipitated by slow addition of 50 ml of water
4. filtrationcollected by filtration
5. washThe crystals were washed with water
6. customsucked dry
7. washwashed with methanol/ether
8. customto leave light yellow product
9. extractionextracted with methylene chloride
10. washThe extracts were washed with water
11. customdried
12. customevaporated
13. customCrystallization of the residue from methylene chloride/hexane yielded additional product
14. customThe analytical sample was recrystallized from ether
15. customto give pale yellow crystals with mp 220°-230° C. dec.