1,4-Dioxane hydrochloride → HCID 178465606, compound

HRID 361732Notes

Reaction equation

HRID 361732 reaction equation
C(OC([NH:8][CH2:9][C:10]#[C:11][CH2:12][NH:13][C:14](=[NH:16])[CH3:15])=O)CCC.Cl.O1CCOCC1>>[NH2:8][CH2:9][C:10]#[C:11][CH2:12][NH:13][C:14](=[NH:16])[CH3:15]

Participants

3

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 178453446HCID 178453446, compound

Product 1

HCID 178465606HCID 178465606, compound

Procedure

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.

Workup

  1. customAfter this time the mother liquor was decanted off
  2. customto remove residual solvent
  3. customThe resulting material was triturated with dry diethyl ether (×2)
  4. filtrationfiltered off
  5. washwashed with more dry diethyl ether
  6. customThe yellow solid was finally dried in a drying pistol

Sources & evidence

ORD record
ord-99eb5985c282493da86cd39617360bd6
Source dataset
uspto-grants-1999_02
Patent number
US05866612

Reaction notes

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