1,4-Dioxane hydrochloride → HCID 67380985, compound

HRID 2409407Notes

Reaction equation

HRID 2409407 reaction equation
[CH2:1]([N:4]1[CH2:9][CH2:8][CH:7]([O:10][C:11]2[CH:25]=[CH:24][C:14]3[NH:15][C:16](=[O:23])[C:17]4[CH2:18][CH2:19][CH2:20][NH:21][C:22]=4[C:13]=3[CH:12]=2)[CH2:6][CH2:5]1)[CH2:2][CH3:3].O1CCOCC1.[ClH:32]>C(O)C.O1CCOCC1>[ClH:32].[ClH:32].[CH2:1]([N:4]1[CH2:9][CH2:8][CH:7]([O:10][C:11]2[CH:25]=[CH:24][C:14]3[NH:15][C:16](=[O:23])[C:17]4[CH2:18][CH2:19][CH2:20][NH:21][C:22]=4[C:13]=3[CH:12]=2)[CH2:6][CH2:5]1)[CH2:2][CH3:3]

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 58424877HCID 58424877, compound

Product 1

HCID 67380985HCID 67380985, compoundYield 79%

Reagents, catalysts & solvents 1

HCID 22560076Dioxan ethanolSolvent

Procedure

The compound (28 mg, 0.08 mmol) prepared in step 6 was dissolved in ethanol/1,4-dioxane, added with 3.7 N hydrochloric acid 1,4-dioxane solution. The resulting mixture was stirred overnight at room temperature. Once the reaction was completed, the mixture was concentrated under reduced pressure and washed with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to obtain the title compound (27 mg, yield: 79%, yellow solid).

Workup

  1. concentrationthe mixture was concentrated under reduced pressure
  2. washwashed with ethyl acetate
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-a4467719989f40708f5cb575fc4ff7a2
Source dataset
uspto-grants-2014_08
Patent number
US08815891B2

Reaction notes

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