Hydrochloric Acid → HCID 9944441, compound

HRID 496078Notes

Reaction equation

HRID 496078 reaction equation
[CH3:1][N:2]([C:10]1([CH2:13][CH2:14][O:15][C:16]2[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=2)[CH2:12][CH2:11]1)C(=O)OC(C)(C)C.Cl.[C:23]([O-:30])(=[O:29])/[CH:24]=[CH:25]/[C:26]([O-:28])=[O:27].C(O)(=O)/C=C/C(O)=O>O1CCOCC1.CCOCC>[C:23]([OH:30])(=[O:29])/[CH:24]=[CH:25]/[C:26]([OH:28])=[O:27].[CH3:1][NH:2][C:10]1([CH2:13][CH2:14][O:15][C:16]2[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=2)[CH2:11][CH2:12]1

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 444972Fumaric AcidHCID 5460307FumarateHCID 17840525HCID 17840525, compound

Product 1

HCID 9944441HCID 9944441, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 312751,4-DioxaneSolvent2×

Procedure

A solution of 1.2 g of the product obtained in Step 1 dissolved in 5 ml of dioxane and 4 ml of 4N hydrochloric acid in dioxan is stirred for 20 hours at ambient temperature and then 10 ml of ether are added. The precipitate formed is separated off, taken up in 15 ml of water and made alkaline by the addition of potassium carbonate. The aqueous phase is then extracted with dichloromethane. The organic phases are subjected to customary treatment which, after concentration under reduced pressure, allows the expected product to be obtained, which is converted into its fumarate form by treatment with an ethanolic solution of fumaric acid.

Workup

  1. customThe precipitate formed
  2. customis separated off
  3. additionby the addition of potassium carbonate
  4. extractionThe aqueous phase is then extracted with dichloromethane
  5. concentrationafter concentration under reduced pressure
  6. customto be obtained

Sources & evidence

ORD record
ord-9d33c96ecabb44f3a5617fd0542f40a4
Source dataset
uspto-grants-2005_09
Patent number
US06943184B2

Reaction notes

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