1,4-Dioxane hydrochloride → HCID 23155392, compound

HRID 2080884Notes

Reaction equation

HRID 2080884 reaction equation
C(OC(=O)[NH:7][CH2:8][CH2:9][O:10][CH2:11][CH2:12][N:13]([CH2:17][CH2:18][CH3:19])[CH2:14][CH2:15][CH3:16])(C)(C)C.Cl.O1CCOCC1>CO>[NH2:7][CH2:8][CH2:9][O:10][CH2:11][CH2:12][N:13]([CH2:17][CH2:18][CH3:19])[CH2:14][CH2:15][CH3:16]

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 86614916HCID 86614916, compound

Product 1

HCID 23155392HCID 23155392, compoundYield 96.9%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

The compound (128 mg) obtained in Example 90-2 was dissolved in anhydrous methanol (2.0 ml) and added with a 4 mol/l hydrogen chloride/dioxane solution (2.00 ml) and the whole was stirred at room temperature for 2 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 (81.0 mg) as a colorless oily substance.

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-6b3f5c4cf5e44650b63aec08c3f8e6ad
Source dataset
uspto-grants-2011_04
Patent number
US07932281B2

Reaction notes

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