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Hydrochloric Acid → HCID 178527520, compound

HRID 1505553
Notes
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Reaction equation

HRID 1505553 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[C:44]2[O:43][CH2:42][CH2:41][C:40]=2[CH:39]=[CH:38][CH:37]=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[C:44]5[O:43][CH2:42][CH2:41][C:40]=5[CH:39]=[CH:38][CH:37]=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
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 86702981HCID 86702981, compound

Product 1

HCID 178527520HCID 178527520, 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)-2,3-dihydrobenzofuran-7-sulfonamide (20 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
  • extractionAfter extraction with ethylacetate
  • dry with materialthe organic layer was dried with sulfuric anhydride magnesium and vacuum
  • concentrationconcentrated
  • customwas obtained
  • Sources & evidence

    ORD record
    ord-c3a4dc220d2949c9b37558b0c9d41ec4
    Source dataset
    uspto-grants-2015_12
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US09216981B2

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes