반응 #45029

반응 방정식

Potassium hydroxide

5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine

(2-Methylpropan-2-yl)oxycarbonyl tert-butyl carbonate

→

tert-butyl 5-amino-3-[(3,5-dimethoxyphenyl)methoxy]pyrazole-1-carboxylate

수율 99.0%

용매

water

DCM

dichloromethane

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타The reaction mixture was separated
3. 3
   세척the organic layer was washed with water (2×15 ml), brine (2×15 ml)
4. 4
   건조dried over sodium sulphate
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타dried in vacuo

실험 절차

Potassium hydroxide (11.19 g, 199.4 mmol) dissolved in water (44.8 ml) was added to a solution of 5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine (7.121 g) dissolved in dichloromethane (40 ml). (2-Methylpropan-2-yl)oxycarbonyl tert-butyl carbonate (6.8 g, 31.2 mmol) dissolved in DCM (35 ml) was added and the reaction mixture was stirred vigorously at room temperature for 4 h. The reaction mixture was separated and the organic layer was washed with water (2×15 ml), brine (2×15 ml), dried over sodium sulphate, filtered, evaporated and dried in vacuo to give tert-butyl 5-amino-3-[(3,5-dimethoxyphenyl)methoxy]pyrazole-1-carboxylate (8.70 g, 99%) as a cream solid.

출처