Hydrochloric Acid → HCID 69923090, compound

HRID 2415106Notes

Reaction equation

HRID 2415106 reaction equation
C([O:8][C:9]1[CH:25]=[CH:24][C:12]([CH2:13][NH:14][C:15]2[C:20]([Cl:21])=[C:19](C)[N:18]=[C:17]([CH3:23])[N:16]=2)=[CH:11][C:10]=1[O:26][CH:27]([F:29])[F:28])C1C=CC=CC=1.Cl.[CH2:31](O)C>>[Cl:21][C:20]1([CH3:31])[CH:19]=[N:18][C:17]([CH3:23])=[N:16][CH:15]1[NH:14][CH2:13][C:12]1[CH:24]=[CH:25][C:9]([OH:8])=[C:10]([O:26][CH:27]([F:28])[F:29])[CH:11]=1

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 22640007HCID 22640007, compound

Product 1

HCID 69923090HCID 69923090, compoundYield 41%

Procedure

In analogy to the method described in example B1, 6.9 g (16.4 mmol) of [4-benzyloxy-3-(1.1-difluoromethoxy)benzyl](5-chloro-2,6-dimethylpyrimidin-4-yl)amine (from example A6) are reacted with 70 ml of 12.5N hydrochloric acid in 70 ml of ethanol. Extraction with ethyl acetate at a pH of 8 gives, after concentration, a solid residue. Extraction by stirring with petroleum ether and drying give 2.2 g (41%) of the title compound as a beige crystallizate. m.p.: 167-168.5° C.

Workup

  1. extractionExtraction with ethyl acetate at a pH of 8
  2. customgives
  3. concentrationafter concentration
  4. extractionExtraction
  5. customdrying

Sources & evidence

ORD record
ord-aa65d176c8ce4c0cbebe7f4b89afad11
Source dataset
uspto-grants-2004_11
Patent number
US06818642B2

Reaction notes

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