反応 #215032

反応方程式

7-Chloro-5-(2-fluorophenyl)-1,3-dihydro-2-nitromethylene-2H-1,4-benzodiazepine-4-oxide

sodium nitrite

sodium nitrite

→

7-Chloro-5-(2-fluorophenyl)-N-hydroxy-α-nitro-3H-1,4 -benzodiazepine-2-methanimine 4-oxide

溶媒

acetic acid

water

water

反応条件

後処理

1. 1
   workup.DISSOLUTIONwas dissolved
2. 2
   その他reached 70° C.
3. 3
   温度while cooling
4. 4
   workup.ADDITIONthe addition
5. 5
   抽出extracted with methylene chloride
6. 6
   洗浄The extracts were washed with water
7. 7
   乾燥dried over sodium sulfate
8. 8
   その他evaporated
9. 9
   その他Crystallization of the residue from ethyl acetate yielded yellow crystals

実験手順

7-Chloro-5-(2-fluorophenyl)-1,3-dihydro-2-nitromethylene-2H-1,4-benzodiazepine-4-oxide* 7 g (0.02 mole), was dissolved by heating in 250 ml of glacial acetic acid. The solution was cooled with tap water and when the temperature reached 70° C. the addition of 1.9 g (0.0275 mole) of sodium nitrite was started. The sodium nitrite was added over a period of 10 min while cooling was continued. Following the addition, the mixture was stirred for 11/2 hr at room temperature, diluted with water and extracted with methylene chloride. The extracts were washed with water, dried over sodium sulfate and evaporated. Crystallization of the residue from ethyl acetate yielded yellow crystals.

出典