HCID 68180982, compound → HCID 68181121, compound

HRID 2167098Notes

Reaction equation

HRID 2167098 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1[CH2:14][CH2:15][N:16]([CH:23]1[CH2:31][C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH2:24]1)[C:17]1[N:22]=[CH:21][CH:20]=[CH:19][N:18]=1)=O)(C)(C)C>Cl.O1CCOCC1>[CH2:24]1[C:25]2[C:30](=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:31][CH:23]1[N:16]([C:17]1[N:18]=[CH:19][CH:20]=[CH:21][N:22]=1)[CH2:15][CH2:14][CH:9]1[CH2:10][CH2:11][CH2:12][CH2:13][NH:8]1

Participants

3

Reactant 1

HCID 68180982HCID 68180982, compound

Product 1

HCID 68181121HCID 68181121, compound

Reagents, catalysts & solvents 1

HCID 204431481,4-Dioxane hydrochlorideSolvent

Procedure

To compound 47 (0.303 g, 0.72 mmol) was added dioxane-HCl (20 mL) at ice-cold condition and the solution was stirred for 4 hours at rt. The solution was then concentrated under reduced pressure and dissolved in ethyl acetate. The organic layer was washed with saturated NaHCO3 solution, water and brine, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to provide sticky compound 48.

Workup

  1. concentrationThe solution was then concentrated under reduced pressure
  2. dissolutiondissolved in ethyl acetate
  3. washThe organic layer was washed with saturated NaHCO3 solution, water and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-98f0157843e34f6aa79e3af09530147e
Source dataset
uspto-grants-2015_06
Patent number
US09044482B2

Reaction notes

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