Sodium Bicarbonate → HCID 87189364, compound

HRID 1893574Notes

Reaction equation

HRID 1893574 reaction equation
C(OC(=O)[NH:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][C:17]=1[CH3:18])[N:14]([CH2:19][CH:20]([F:22])[F:21])[C:13](=[O:23])[CH2:12][CH2:11]2)(C)(C)C.Cl.O1CCOCC1.C(=O)([O-])O.[Na+]>ClCCl>[NH2:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][C:17]=1[CH3:18])[N:14]([CH2:19][CH:20]([F:22])[F:21])[C:13](=[O:23])[CH2:12][CH2:11]2

Participants

5

Reactant 3

HCID 516892Sodium BicarbonateHCID 204431481,4-Dioxane hydrochlorideHCID 123780276HCID 123780276, compound

Product 1

HCID 87189364HCID 87189364, compoundYield 88.4%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

The compound (2.29 g, 6.73 mmol) of step C was dissolved in dichloromethane (15 ml), 4N hydrochloric acid-dioxane solution (15 ml, 60 mmol) was added at room temperature, and the mixture was stirred at the same temperature for 2 hr. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate, the mixture was extracted with ethyl acetate, and the organic layer was dried over saturated brine. The insoluble material was filtered off, and the solution was concentrated under reduced pressure to give the title compound (1.43 g, yield 88%) as a colorless solid.

Workup

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialthe organic layer was dried over saturated brine
  3. filtrationThe insoluble material was filtered off
  4. concentrationthe solution was concentrated under reduced pressure

Sources & evidence

ORD record
ord-6544070056194e20b957948130899e3d
Source dataset
uspto-grants-2013_08
Patent number
US08513235B2

Reaction notes

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