反应 #89793

反应方程式

3-hydrazinobenzoic acid

isopropylmethylketone

→

product

收率 81.4%

2,3,3-Trimethyl-4-carboxy-3H-indole

收率 81.4%

溶剂

ethanol

sulfuric acid

反应条件

后处理

1. 1
   温度under reflux in an oil bath for 20 h
2. 2
   其他was evaporated off under reduced pressure to a small volume of ˜200 mL
3. 3
   其他Collected the solid with a filter funnel
4. 4
   洗涤washed with iPrOH (3×30 mL) and ethyl ether (3×30 mL)
5. 5
   其他dried
6. 6
   其他Further drying of the solid in an oven at 45° C. under high vacuum for 18 h

实验过程

A solution of 3-hydrazinobenzoic acid (30.0 g, 197 mmol), isopropylmethylketone (31.7 mL, 296 mmol) in ethanol (500 mL) and sulfuric acid (5 mL) was heated under reflux in an oil bath for 20 h. After cooling to ambient temperature the solvent was evaporated off under reduced pressure to a small volume of ˜200 mL. Collected the solid with a filter funnel, washed with iPrOH (3×30 mL) and ethyl ether (3×30 mL) and dried. Further drying of the solid in an oven at 45° C. under high vacuum for 18 h provided 32.59 g (81.3%) of the product. (This is [0148]1.2)

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