반응 #2287239

반응 방정식

(2-methoxyethyl) hydrazine oxalic acid

4,4-dimethyl-3-oxopentanenitrile

→

title compound

수율 98.5%

5-tert-Butyl-2-(2-methoxyethyl)-2H-pyrazol-3-ylamine

수율 98.5%

용매

ethanol

반응 조건

후처리

1. 1
   workup.DISSOLUTIONdissolved
2. 2
   온도to cool overnight
3. 3
   기타the solvent was evaporated
4. 4
   workup.DISSOLUTIONThe residue was dissolved in dichloromethane (20 mL)
5. 5
   세척washed with saturated aqueous NaHCO3 (10 mL)
6. 6
   기타The organic layer was separated
7. 7
   기타evaporated
8. 8
   workup.DISSOLUTIONThe residual oil was dissolved in diethyl ether
9. 9
   기타evaporated

실험 절차

A stirred suspension of (2-methoxyethyl) hydrazine oxalic acid (0.50 g, 2.77 mmol) and 4,4-dimethyl-3-oxopentanenitrile (0.347 g, 2.77 mmol) in ethanol (6 mL) was heated at 85° C. for 4.5 h during which time all solids dissolved. The reaction mixture was allowed to cool overnight and then the solvent was evaporated. The residue was dissolved in dichloromethane (20 mL) and washed with saturated aqueous NaHCO3 (10 mL). The organic layer was separated using a phase separator cartridge and evaporated. The residual oil was dissolved in diethyl ether and evaporated to afford the title compound (0.538 g, 98%) as a solid. 1H NMR (300 MHz, CDCl3): 1.26 (9H, s), 3.33 (3H, s), 3.67 (2H, t, J 4.3 Hz), 3.95 (2H, br s), 4.13 (2H, t, J 4.6 Hz), 5.36 (1H, s).

출처