Hydrochloric Acid → HCID 136388585, compound

HRID 131473Notes

Reaction equation

HRID 131473 reaction equation
[F:1][C:2]1[C:3]([F:27])=[CH:4][C:5]2[N:14]=[C:13]([N:15]3[CH2:20][CH2:19][N:18]([CH3:21])[C@@H:17]([CH2:22][CH2:23][OH:24])[CH2:16]3)[C:12]3[CH:11]=[C:10]([CH3:25])[S:9][C:8]=3[NH:7][C:6]=2[CH:26]=1.[ClH:28]>C(OCC)(=O)C.C(O)C>[ClH:28].[ClH:28].[F:1][C:2]1[C:3]([F:27])=[CH:4][C:5]2[N:14]=[C:13]([N:15]3[CH2:20][CH2:19][N:18]([CH3:21])[C@@H:17]([CH2:22][CH2:23][OH:24])[CH2:16]3)[C:12]3[CH:11]=[C:10]([CH3:25])[S:9][C:8]=3[NH:7][C:6]=2[CH:26]=1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 136090355HCID 136090355, compound

Product 1

HCID 136388585HCID 136388585, compoundYield 98%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

Dissolve (S)-2-[4-(6,7-difluoro-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulen-10-yl)-1-methyl-piperazin-2-yl]-ethanol (171 mg, 0.44 mmol) in ethyl acetate. Add 3 equivlents of hydrogen chloride in ethanol. After 18 hours filter the precipitate under a nitrogen atmosphere, wash with ethyl acetate and dry under vacuum to give the title compound (198 mg, 98%): Mass Spectrum (LCMS) 393 (M+1); 391 (M−1).

Workup

  1. filtrationAfter 18 hours filter the precipitate under a nitrogen atmosphere
  2. washwash with ethyl acetate
  3. customdry under vacuum

Sources & evidence

ORD record
ord-14d2c8381558407e9138f7335d4f55b8
Source dataset
uspto-grants-2008_06
Patent number
US07384934B2

Reaction notes

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