1,4-Dioxane hydrochloride → HCID 66818214, compound

HRID 1754900Notes

Reaction equation

HRID 1754900 reaction equation
[ClH:1].O1CCOCC1.C(OC([N:15]1[CH2:33][CH2:32][C:18]2([N:22]=[C:21]([C:23]3[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:24]=3[Cl:30])[NH:20][C:19]2=[O:31])[CH2:17][CH2:16]1)=O)(C)(C)C>C(Cl)Cl.C(Cl)Cl.CCCCCC>[ClH:29].[ClH:1].[Cl:30][C:24]1[CH:25]=[C:26]([Cl:29])[CH:27]=[CH:28][C:23]=1[C:21]1[NH:20][C:19](=[O:31])[C:18]2([CH2:32][CH2:33][NH:15][CH2:16][CH2:17]2)[N:22]=1

Participants

5

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 66817079HCID 66817079, compound

Product 1

HCID 66818214HCID 66818214, compoundYield 219.4%

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 21226440Methylenechloride HexaneSolvent

Procedure

4 N HCl-dioxane (20 ml, 80 mmol) was added to a solution of 2-(2,4-dichloro-phenyl)-4-oxo-1,3,8-triaza-spiro[4.5]dec-1-ene-8-carboxylic acid tert-butyl ester (3.11 g, 7.81 mmol) in CH2Cl2 (60 mL), and the mixture was stirred at room temperature for four hours. The reaction mixture was diluted with CH2Cl2-hexane, and the precipitated solid was then filtered. The resulting solid was washed with ethyl acetate and then dried under reduced pressure to give 2-(2,4-dichloro-phenyl)-1,3,8-triaza-spiro[4.5]dec-1-en-4-one dihydrochloride (3.18 g) as a colorless solid.

Workup

  1. filtrationthe precipitated solid was then filtered
  2. washThe resulting solid was washed with ethyl acetate
  3. customdried under reduced pressure

Sources & evidence

ORD record
ord-58b1694a638e4100ad276a207bedab63
Source dataset
uspto-grants-2015_10
Patent number
US09169254B2

Reaction notes

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