反応 #497304

反応方程式

N-(4-fluoro-3-chloro-phenyl)-2-fluoro-4-methylamino-5-nitro-benzoic acid amide

2-fluoroethanol

2-fluoroethanol

KHMDS

KHMDS

→

N-(3-chloro-4-fluorophenyl)-2-(2-fluoroethoxy)-4-methylamino-5-nitro-benzamide

溶媒

THF

反応条件

後処理

1. 1
   温度cooled
2. 2
   workup.STIRRINGit is stirred for 4.5 h at 60° C
3. 3
   workup.ADDITIONThen the mixture is diluted with satd
4. 4
   ろ過aq. NaHCO3-solution and the precipitate is filtered off
5. 5
   洗浄washed with water
6. 6
   その他dried

実験手順

KHMDS (0.320 g, 1.60 mmol) is added to an ice-cooled mixture of N-(4-fluoro-3-chloro-phenyl)-2-fluoro-4-methylamino-5-nitro-benzoic acid amide (500 mg, 1.46 mmol), 2-fluoroethanol (0.129 ml, 2.19 mmol) and 30 ml THF. After 30 min the temperature is raised to 60° C. for 4.5 h, then it is stirred at rt overnight. Additional 2-fluoroethanol (0.129 ml, 2.19 mmol) and KHMDS (0.160 g, 0.80 mmol) are added and it is stirred for 4.5 h at 60° C. Then the mixture is diluted with satd. aq. NaHCO3-solution and the precipitate is filtered off, washed with water and dried.

出典