1,4-Dioxane hydrochloride → HCID 66882050, compound

HRID 1893565Notes

Reaction equation

HRID 1893565 reaction equation
[CH2:1]([O:3][C:4](=[O:29])[CH2:5][N:6]([CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[C:7]1[CH:12]=[C:11]([CH2:13][CH2:14][C:15]([O:17]C(C)(C)C)=[O:16])[CH:10]=[CH:9][C:8]=1[CH3:22])[CH3:2].Cl.O1CCOCC1>ClCCl>[CH2:1]([O:3][C:4](=[O:29])[CH2:5][N:6]([CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[C:7]1[CH:12]=[C:11]([CH2:13][CH2:14][C:15]([OH:17])=[O:16])[CH:10]=[CH:9][C:8]=1[CH3:22])[CH3:2]

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 66882028HCID 66882028, compound

Product 1

HCID 66882050HCID 66882050, compoundYield 79%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

To dichloromethane (8.8 ml) were added the compound (1.79 g, 4.40 mmol) obtained in step B and 4N hydrochloric acid-dioxane solution (8.8 ml), and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with dichloromethane, washed with water, and dried over sodium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure. The obtained oil was purified by silica gel column chromatography (ethyl acetate-hexane) to give the title compound (1.21 g, yield 79%) as a colorless oil.

Workup

  1. washwashed with water
  2. dry with materialdried over sodium sulfate
  3. filtrationThe insoluble material was filtered off
  4. concentrationthe solution was concentrated under reduced pressure
  5. customThe obtained oil was purified by silica gel column chromatography (ethyl acetate-hexane)

Sources & evidence

ORD record
ord-348f109421c749e69e3d451919c071f4
Source dataset
uspto-grants-2013_08
Patent number
US08513235B2

Reaction notes

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