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Ammonium Chloride → N-{[6-(4,4-dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidin-4-yl]methyl}tetrahydro-2H-thiopyran-4-amine-1,1-dioxide hydrochloride

HRID 2171826
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Reaktionsgleichung

Reaktionsgleichung von HRID 2171826
CS(O[CH2:6][C:7]1[C:8]2[CH:16]=[C:15]([CH:17]3[CH2:22][CH2:21][C:20]([CH3:24])([CH3:23])[CH2:19][CH2:18]3)[S:14][C:9]=2[N:10]=[C:11]([CH3:13])[N:12]=1)(=O)=O.CCN(C(C)C)C(C)C.[S:34]1(=[O:42])(=[O:41])[CH2:39][CH2:38][CH:37]([NH2:40])[CH2:36][CH2:35]1.[NH4+].[Cl-:44]>CN(C=O)C>[ClH:44].[CH3:23][C:20]1([CH3:24])[CH2:21][CH2:22][CH:17]([C:15]2[S:14][C:9]3[N:10]=[C:11]([CH3:13])[N:12]=[C:7]([CH2:6][NH:40][CH:37]4[CH2:38][CH2:39][S:34](=[O:42])(=[O:41])[CH2:35][CH2:36]4)[C:8]=3[CH:16]=2)[CH2:18][CH2:19]1
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Komponenten

6

Edukt 4

HCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 4188082H-Thiopyran-4-amine, tetrahydro-, 1,1-dioxideHCID 118023751[6-(4,4-Dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidin-4-yl]methyl methanesulfonate

Produkt 1

HCID 118023896N-{[6-(4,4-dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidin-4-yl]methyl}tetrahydro-2H-thiopyran-4-amine-1,1-dioxide hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a mixture of [6-(4,4-dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidin-4-yl]methyl methanesulfonate (200 mg), DIPEA (139 μL), and DMF (3.0 mL) was added tetrahydro-2H-thiopyran-4-amine-1,1-dioxide (97 mg), followed by stirring at room temperature for 4 hours. To the reaction mixture was added a saturated aqueous NH4Cl solution, followed by extraction with EtOAc. The organic layer was washed sequentially with water and brine, dried over MgSO4, and then concentrated under reduced pressure. The residue was purified by silica gel column and dissolved in EtOAc, and 4 M HCl/EtOAc (137 μL) was added dropwise. The precipitate was collected by filtration and then dried to obtain N-{[6-(4,4-dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidin-4-yl]methyl}tetrahydro-2H-thiopyran-4-amine-1,1-dioxide hydrochloride (165 mg).

Aufarbeitung

  1. extractionfollowed by extraction with EtOAc
  2. washThe organic layer was washed sequentially with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column
  6. dissolutiondissolved in EtOAc
  7. addition4 M HCl/EtOAc (137 μL) was added dropwise
  8. filtrationThe precipitate was collected by filtration
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-97ac3c20b7f2463e8493a1e353283fd7
Quelldatensatz
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09051339B2

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