반응 #514364

반응 방정식

1-Butoxycarbonylamino-4-(1-imino-2-fluoroethylamino) but-2-yne hydrobromide

HBr

→

1-amino-4-(1-imino-2-fluoroethylamino)but-2-yne dihydrobromide

용매

acetic acid

acetic acid

반응 조건

후처리

1. 1
   온도cooling until the solution
2. 2
   온도with cooling for 1 h
3. 3
   기타After this time the mother liquor was decanted off
4. 4
   기타to remove residual solvent
5. 5
   기타The resulting material was triturated with dry diethyl ether (×2)
6. 6
   여과filtered off
7. 7
   세척washed with more dry diethyl ether
8. 8
   기타The yellow solid was recrystallised from ethanol/diethyl ether
9. 9
   기타finally dried in a drying pistol

실험 절차

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.

출처