反应 #40377

ord-a077ae3605094eb692cd00682fc03c6f

反应方程式

[Na+].[OH-]
sodium hydroxide
O=S(=O)(O)O
sulfuric acid
[C-]#N.[Na+]
sodium cyanide
CC(C)=Cc1ccc(F)c(C)c1
1-fluoro-2-methyl-4-(2-methylpropenyl)benzene
Cc1cc(CC(C)(C)NC=O)ccc1F
N-[2-(4-fluoro-3-methylphenyl)-1,1-dimethylethyl]formamide

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with dichloromethane
  2. 2
    干燥The organic phase is dried with sodium sulfate
  3. 3
    其他The slightly yellow oil thus obtained
  4. 4
    其他is further reacted directly

实验过程

4.9 mL concentrated sulfuric acid are added dropwise at 5° C.-15° C. to 1.5 g (31 mmol) sodium cyanide in 5 mL glacial acetic acid. Then the mixture is combined with 3.9 g (24 mmol) of 1-fluoro-2-methyl-4-(2-methylpropenyl)benzene, dissolved in 10 mL glacial acetic acid, and stirred for 1 hour at 50° C.-60° C. The reaction mixture is diluted with ice water, made alkaline with concentrated sodium hydroxide solution, and extracted with dichloromethane. The organic phase is dried with sodium sulfate and freed from solvents in vacuo. The slightly yellow oil thus obtained is further reacted directly. Yield: 4.3 g (87%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07727984B2uspto-grants-2010_06