반응 #514362

반응 방정식

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

HCl dioxane

→

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

반응 조건

후처리

1. 1
   기타After this time the mother liquor was decanted off
2. 2
   기타to remove residual solvent
3. 3
   기타The resulting material was triturated with dry diethyl ether (×2)
4. 4
   여과filtered off
5. 5
   세척washed with more dry diethyl ether
6. 6
   기타The yellow solid was finally dried in a drying pistol

실험 절차

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.

출처