1,4-Dioxane hydrochloride → HCID 67103493, compound

HRID 2080830Notes

Reaction equation

HRID 2080830 reaction equation
[CH2:1]([O:8][C:9](=[O:31])[NH:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16](=O)[N:17]([C:21]1[CH:26]=[C:25]([C:27]#[N:28])[CH:24]=[CH:23][C:22]=1[NH2:29])[CH2:18][CH2:19][CH3:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.O1CCOCC1>CO>[CH2:1]([O:8][C:9](=[O:31])[NH:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[N:17]([CH2:18][CH2:19][CH3:20])[C:21]2[CH:26]=[C:25]([C:27]#[N:28])[CH:24]=[CH:23][C:22]=2[N:29]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 67103581HCID 67103581, compound

Product 1

HCID 67103493HCID 67103493, compoundYield 95.9%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

The compound (317 mg) obtained in Example 48-2 was dissolved in methanol (5.0 ml) and added with a 4 mol/l hydrogen chloride/dioxane solution (2.0 ml) and the whole was stirred for 16 hours. The residue obtained by distilling the solvent off was dissolved in methanol and the solution was neutralized with an anion-exchange resin (Amberlite IRA-410). The resin was filtrated out and the solvent was distilled off, thereby obtaining the subject compound (291 mg) as a colorless oily substance.

Workup

  1. customThe residue obtained
  2. distillationby distilling the solvent
  3. dissolutionoff was dissolved in methanol
  4. filtrationThe resin was filtrated out
  5. distillationthe solvent was distilled off

Sources & evidence

ORD record
ord-d4caae1b0b4d42dbb6cf55933ca34f38
Source dataset
uspto-grants-2011_04
Patent number
US07932281B2

Reaction notes

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