Hydrochloric Acid → HCID 178481183, compound

HRID 1505567Notes

Reaction equation

HRID 1505567 reaction equation
Cl.[F:2][C:3]1[C:8]([NH:9][C:10]2[C:15]([C:16]3[N:24]=[CH:23][N:22]=[C:21]4[C:17]=3[N:18]=[CH:19][N:20]4C3CCCCO3)=[CH:14][CH:13]=[CH:12][N:11]=2)=[C:7]([F:31])[CH:6]=[CH:5][C:4]=1[NH:32][S:33]([C:36]1[CH:37]=[N:38][N:39]([CH3:41])[CH:40]=1)(=[O:35])=[O:34]>>[N:24]1[C:16]([C:15]2[C:10]([NH:9][C:8]3[C:3]([F:2])=[C:4]([NH:32][S:33]([C:36]4[CH:37]=[N:38][N:39]([CH3:41])[CH:40]=4)(=[O:34])=[O:35])[CH:5]=[CH:6][C:7]=3[F:31])=[N:11][CH:12]=[CH:13][CH:14]=2)=[C:17]2[C:21]([NH:20][CH:19]=[N:18]2)=[N:22][CH:23]=1

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 86702988HCID 86702988, compound

Product 1

HCID 178481183HCID 178481183, compound

Procedure

1M aqueous hydrochloric acid solution was added into the N-(2,4-difluoro-3-(3-(9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-yl)pyridin-2-ylamino)phenyl)-1-methyl-1H-pyrazole-4-sulfonamide (19 mg, 0.033 mmol) prepared at Step 10 and stirred for 2 hours. After the reaction, the reactant was washed with an aqueous solution of sodium hydrogen carbonate and salt water. After extraction with ethylacetate, the organic layer was dried with sulfuric anhydride magnesium and vacuum concentrated, and then refined by means of column chromatography, so that the target compound was obtained.

Workup

  1. customprepared at Step 10
  2. customAfter the reaction
  3. washthe reactant was washed with an aqueous solution of sodium hydrogen carbonate and salt water
  4. extractionAfter extraction with ethylacetate
  5. dry with materialthe organic layer was dried with sulfuric anhydride magnesium and vacuum
  6. concentrationconcentrated
  7. customwas obtained

Sources & evidence

ORD record
ord-191d2e220be843f2aab0c1db930da2ce
Source dataset
uspto-grants-2015_12
Patent number
US09216981B2

Reaction notes

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