반응 #89790

반응 방정식

3-hydrazinobenzoic acid

isopropylmethylketone

→

product

수율 81.4%

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

수율 81.4%

용매

ethanol

sulfuric acid

반응 조건

후처리

1. 1
   온도under reflux in an oil bath for 20 h
2. 2
   기타was evaporated off under reduced pressure to a small volume of ˜200 mL
3. 3
   기타Collected the solid with a filter funnel
4. 4
   세척washed with iPrOH (3×30 mL) and ethyl ether (3×30 mL)
5. 5
   기타dried
6. 6
   기타Further drying of the solid in an oven at 45° C. under high vacuum for 18 h

실험 절차

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.

출처