تفاعل #2175457
ord-799709a9e8e04ffc9fff43fe39c09ea1
معادلة التفاعل
9-formyl-2,7-fluorenedicarboxylic acid dibenzyl ester
hydrogen
hydrogen
→
9-formyl-2,7-fluorenedicarboxylic acid
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.ADDITIONthe Parr bottle was evacuated/filled 3 times on a Parr apparatus
- 2أخرىthe remaining hydrogen was removed at reduced pressure
- 3ترشيحThe suspension was filtered over a bed of celite
- 4غسيلrinsed with additional THF
- 5أخرىevaporated
الإجراء التجريبي
In a Parr hydrogenation bottle (Parr Instrument Company, Moline Ill.) was dissolved 9-formyl-2,7-fluorenedicarboxylic acid dibenzyl ester (3.0 g, 0.0061 mol) in THF anh. (350 mL). After careful addition of 20% Pd/C (wet with 50% water) 20% by weight (600 mg), the Parr bottle was evacuated/filled 3 times on a Parr apparatus to ensure hydrogen atmosphere. The suspension was shaken under 20-30 psi hydrogen gas for approximately 60 hours and then the remaining hydrogen was removed at reduced pressure. The suspension was filtered over a bed of celite, rinsed with additional THF and evaporated. 1H-NMR (d6-DMSO): δ (ppm) 9.0 (s, 1H, Ar); 8.5-8.1 (m, 6H, Ar).