تفاعل #6896
ord-941df1acbb1249ef9c18b030f6937c2a
معادلة التفاعل
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىThe resulting mixture was degassed
- 2ترشيحThe reaction mixture was filtered
- 3ترشيحthrough filter aid
- 4أخرىthe solvent removed under vacuum
- 5workup.DISSOLUTIONThe resulting oil was dissolved in ethyl acetate
- 6أخرىthe solvent removed under vacuum
- 7أخرىtriturated until crystallization
- 8ترشيحThe solids were filtered
- 9غسيلwashed with ice-cold ether
- 10أخرىthen dried under vacuum
الإجراء التجريبي
The product of Step A and palladium hydroxide on carbon (1.3 g, 20% by wt) was suspended in methanol (100 mL) and ethyl acetate (100 mL). The resulting mixture was degassed then stirred under hydrogen atmosphere (balloon) for 6 h. The reaction mixture was filtered through filter aid and the solvent removed under vacuum. The resulting oil was dissolved in ethyl acetate and the solvent removed under vacuum. The resulting oil was suspended in ether and triturated until crystallization occurred. The solids were filtered and washed with ice-cold ether then dried under vacuum to afford the product as a brown solid, MS: m/z 254 (MH+), which was used without further purification