反应 #514362

反应方程式

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

HCl dioxane

→

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

反应条件

后处理

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

实验过程

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.

来源