반응 #1929086

반응 방정식

12

Tetramethyl 1-(4-nitrobenzyl)methylenebisphosphonate

→

13

수율 103.4%

Tetramethyl 1-(4-aminobenzyl)methylenebisphosphonate

수율 103.4%

용매

EtOH

반응 조건

후처리

1. 1
   기타The catalyst was removed by filtration through glass fiber
2. 2
   여과filter paper
3. 3
   기타the solvent was removed under reduced pressure

실험 절차

A mixture of 12 (1.01 g, 2.75 mmol) and PtO2 (0.035 g, 0.15 mmol) in EtOH (40 mL, 95%) was shaken in a PARR apparatus under 55 p.s.i of H2 for 14 hr. The catalyst was removed by filtration through glass fiber filter paper and the solvent was removed under reduced pressure to give 13 as a pale yellow solid (0.959 g, 103%) that was used without purification. 1H NMR (400 MHz, CDCl3) δ 2.62 (tt, J=6.3, 23.9, 1H), 3.12 (dt, J=6.3, 16.2, 2H), 3.70 (d, J=1.9, 6H), 3.73 (d, J=1.9, 6H), 6.61 (d, J=8.5, 2H), 7.04 (d, J=8.5, 2H).

출처