反応 #514364
ord-04c226e4c8a34e72ad24d61b137d785c
反応方程式
反応条件
後処理
- 1温度cooling until the solution
- 2温度with cooling for 1 h
- 3その他After this time the mother liquor was decanted off
- 4その他to remove residual solvent
- 5その他The resulting material was triturated with dry diethyl ether (×2)
- 6ろ過filtered off
- 7洗浄washed with more dry diethyl ether
- 8その他The yellow solid was recrystallised from ethanol/diethyl ether
- 9その他finally dried in a drying pistol
実験手順
1-Butoxycarbonylamino-4-(1-imino-2-fluoroethylamino) but-2-yne hydrobromide (500 mg) was deprotected by dissolving in glacial acetic acid (10 ml), cooling until the solution almost solidified and adding HBr in acetic acid (45% wv, 1.8 ml). The mixture was stirred with cooling for 1 h then at room temperature for 1 h. After this time the mother liquor was decanted off and the sticky residue subjected to an oil pump vacuum to remove residual solvent. The resulting material was triturated with dry diethyl ether (×2), filtered off and washed with more dry diethyl ether. The yellow solid was recrystallised from ethanol/diethyl ether and finally dried in a drying pistol to yield 1-amino-4-(1-imino-2-fluoroethylamino)but-2-yne dihydrobromide, Mpt 174°-176.5° C.(dec.), FAB M.S. M+1+144.