反应 #514364

反应方程式

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

HBr

→

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

溶剂

acetic acid

acetic acid

反应条件

后处理

1. 1
   温度cooling until the solution
2. 2
   温度with cooling for 1 h
3. 3
   其他After this time the mother liquor was decanted off
4. 4
   其他to remove residual solvent
5. 5
   其他The resulting material was triturated with dry diethyl ether (×2)
6. 6
   过滤filtered off
7. 7
   洗涤washed with more dry diethyl ether
8. 8
   其他The yellow solid was recrystallised from ethanol/diethyl ether
9. 9
   其他finally dried in a drying pistol

实验过程

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.

来源