반응 #1685
ord-e27f2076ea2944b58cddfe057fe8345b
반응 방정식
1-isoquinolinecarboxylic acid
hydrogen
→
perhydro-1-isoquinolinecarboxylic acid
수율 56.8%
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과The reaction mixture was filtered through a pad of diatomaceous earth
- 2농축the filtrate was concentrated in vacuo
- 3기타The solid was triturated with water
- 4여과filtered
- 5기타dried
실험 절차
A solution of 1-isoquinolinecarboxylic acid (50 g, 0.288 mol) in EtOH (150 mL) and 60 mL of 5N HCl was reduced over 5% Rh/Al2O3 (14 g) at 52 bar (750 psi) of hydrogen in a high pressure apparatus at 50° C. for 17 hours. The reaction mixture was filtered through a pad of diatomaceous earth, and the filtrate was concentrated in vacuo. The solid was triturated with water, filtered and dried to give DL-perhydro-1-isoquinolinecarboxylic acid (DL-1-Piq-OH) (30 g, 48%) FD-MS 184 (MH+).