1,4-Dioxane hydrochloride → HCID 67381151, compound

HRID 2409397Notes

Reaction equation

HRID 2409397 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[C:15]3[NH:14][CH2:13][CH2:12][CH2:11][C:10]=3[C:9](=[O:16])[NH:8][C:7]=2[CH:17]=1.O1CCOCC1.[ClH:24]>O1CCOCC1>[ClH:24].[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[C:15]3[NH:14][CH2:13][CH2:12][CH2:11][C:10]=3[C:9](=[O:16])[NH:8][C:7]=2[CH:17]=1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 58424842HCID 58424842, compound

Product 1

HCID 67381151HCID 67381151, compoundYield 56.9%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

The compound (57.8 mg, 0.251 mmol) prepared in step 5 was dissolved in 1,4-dioxane (1 ml), added with 3.6N hydrochloric acid 1,4-dioxane solution (1 ml) and then stirred for 24 hours. Once the reaction was completed, the solvent was removed under reduced pressure and accordingly obtained residue was stirred for 30 minutes in ethyl acetate/diethyl ether. The resultant solid was filtered and washed with diethyl ether to obtain the title compound (38.1 mg, yield: 56.9%, green solid).

Workup

  1. customthe solvent was removed under reduced pressure and accordingly obtained residue
  2. stirringwas stirred for 30 minutes in ethyl acetate/diethyl ether
  3. filtrationThe resultant solid was filtered
  4. washwashed with diethyl ether

Sources & evidence

ORD record
ord-082d44e56e294519aa537fdedf9596b2
Source dataset
uspto-grants-2014_08
Patent number
US08815891B2

Reaction notes

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