تفاعل #514362

ord-8e6c983dc5e24cb68195a64dd61361a5

معادلة التفاعل

CCCCOC(=O)NCC#CCNC(C)=N
1-Butoxycarbonylamino-4-(1-iminoethylamino)but-2-yne
C1COCCO1.Cl
HCl dioxane
CC(=N)NCC#CCN
1-amino-4-(1-iminoethylamino)but-2-yne

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter this time the mother liquor was decanted off
  2. 2
    أخرىto remove residual solvent
  3. 3
    أخرىThe resulting material was triturated with dry diethyl ether (×2)
  4. 4
    ترشيحfiltered off
  5. 5
    غسيلwashed with more dry diethyl ether
  6. 6
    أخرىThe yellow solid was finally dried in a drying pistol

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: USRE037438E1uspto-grants-2001_11