反应 #80917

反应方程式

2-amino-5-(trimethylsilylethynyl)-6-methylbenzonitrile

potassium carbonate

→

2-amino-5-ethynyl-6-methylbenzonitrile

收率 106.7%

溶剂

methanol

反应条件

后处理

1. 1
   浓缩The reaction mixture was then concentrated under reduced pressure to a residue
2. 2
   萃取the solution was extracted with two 200 mL portions of diethyl ether
3. 3
   干燥The combined extracts were dried with magnesium sulfate
4. 4
   过滤filtered
5. 5
   浓缩The filtrate was concentrated under reduced pressure

实验过程

A mixture of 1.4 grams (0.006 mole) of 2-amino-5-(trimethylsilylethynyl)-6-methylbenzonitrile and 0.9 gram (0.006 mole) of potassium carbonate in 50 mL of methanol was stirred at ambient temperature for one hour. The reaction mixture was then concentrated under reduced pressure to a residue. The residue was taken up in about 75 mL of water, and the solution was extracted with two 200 mL portions of diethyl ether. The combined extracts were dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure, yielding 1.0 gram of 2-amino-5-ethynyl-6-methylbenzonitrile. The NMR spectrum was consistent with the proposed structure. This reaction was repeated several times.

来源