反応 #990286

反応方程式

diazomethane

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

→

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

溶媒

ether

methylene chloride

反応条件

後処理

1. 1
   その他resulted
2. 2
   その他The excess diazomethane was destroyed by addition of acetic acid
3. 3
   洗浄The reaction mixture was washed with aqueous sodium bicarbonate solution
4. 4
   乾燥dried over sodium sulfate
5. 5
   その他evaporated
6. 6
   その他Crystallization of the residue from ether yielded yellow crystals
7. 7
   その他The analytical sample was recrystallized from ether, mp 207°-209°

実験手順

A solution of diazomethane in ether was added to a suspension of 3.8 g (0.01 mol) of 7-chloro-5-(2-fluorophenyl)-N-hydroxy-α-nitro-3H-1,4-benzodiazepine-2-methanimine 4-oxide in 200 ml of methylene chloride. The mixture was stirred for 1 hr at room temperature whereby a clear solution resulted. The excess diazomethane was destroyed by addition of acetic acid. The reaction mixture was washed with aqueous sodium bicarbonate solution, dried over sodium sulfate and evaporated. Crystallization of the residue from ether yielded yellow crystals. The analytical sample was recrystallized from ether, mp 207°-209°.

出典