1,4-Dioxane hydrochloride → HCID 23155537, compound

HRID 2080826Notes

Reaction equation

HRID 2080826 reaction equation
C(OC(=O)[NH:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12](=O)[N:13]([C:17]1[CH:22]=[C:21]([C:23]#[N:24])[CH:20]=[CH:19][C:18]=1[NH2:25])[CH:14]([CH3:16])[CH3:15])(C)(C)C.Cl.O1CCOCC1>CO>[NH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]1[N:13]([CH:14]([CH3:16])[CH3:15])[C:17]2[CH:22]=[C:21]([C:23]#[N:24])[CH:20]=[CH:19][C:18]=2[N:25]=1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 67103841HCID 67103841, compound

Product 1

HCID 23155537HCID 23155537, compoundYield 86.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

The compound (44.1 mg) obtained in Example 47-1 was dissolved in anhydrous methanol (1.0 ml) and added with a 4 mol/l hydrogen chloride/dioxane solution (1.0 ml) and the whole was stirred at room temperature for 3 hours. After completion of the reaction, the solvent was distilled off. The resultant was added with a 1 mol/l sodium hydroxide aqueous solution and the whole was subjected to extraction with chloroform and washed with a saturated saline solution. The organic layer was dried with anhydrous sodium sulfate. The solvent was distilled off, thereby obtaining the subject compound (26.0 mg) as a white crystal.

Workup

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off
  3. additionThe resultant was added with a 1 mol/l sodium hydroxide aqueous solution
  4. extractionthe whole was subjected to extraction with chloroform
  5. washwashed with a saturated saline solution
  6. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  7. distillationThe solvent was distilled off

Sources & evidence

ORD record
ord-5b4a75bb448a487ca74d4dd538288bb4
Source dataset
uspto-grants-2011_04
Patent number
US07932281B2

Reaction notes

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