تفاعل #514364

معادلة التفاعل

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

HBr

→

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

المذيبات

acetic acid

acetic acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooling until the solution
2. 2
   درجة الحرارةwith cooling for 1 h
3. 3
   أخرىAfter this time the mother liquor was decanted off
4. 4
   أخرىto remove residual solvent
5. 5
   أخرىThe resulting material was triturated with dry diethyl ether (×2)
6. 6
   ترشيحfiltered off
7. 7
   غسيلwashed with more dry diethyl ether
8. 8
   أخرىThe yellow solid was recrystallised from ethanol/diethyl ether
9. 9
   أخرىfinally dried in a drying pistol

الإجراء التجريبي

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.

المصدر