反応 #514362

反応方程式

1-Butoxycarbonylamino-4-(1-iminoethylamino)but-2-yne

HCl dioxane

→

1-amino-4-(1-iminoethylamino)but-2-yne

反応条件

後処理

1. 1
   その他After this time the mother liquor was decanted off
2. 2
   その他to remove residual solvent
3. 3
   その他The resulting material was triturated with dry diethyl ether (×2)
4. 4
   ろ過filtered off
5. 5
   洗浄washed with more dry diethyl ether
6. 6
   その他The yellow solid was finally dried in a drying pistol

実験手順

1-Butoxycarbonylamino-4-(1-iminoethylamino)but-2-yne (0.332 g) was deprotected by treatment with 4 N HCl/dioxane (3 ml) at 0° C. and stirring at 0° C. for 1h then at room temperature for 1h. 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 finally dried in a drying pistol to yield 1-amino-4-(1-iminoethylamino)but-2-yne 2.5hydrochloride (0.184 g), Mpt 182°-185° C.(dec), FAB M.S. M+1+126.

出典