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Carbamate → (3R,4R)-3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methyl-N-(pyrimidin-4-yl)piperidine-1-carboxamide

HRID 1969636
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1969636
[C:1](=[O:4])([O-])[NH2:2].Cl.[CH3:6][C@@H:7]1[CH2:12][CH2:11][NH:10][CH2:9][C@@H:8]1[C:13]1[N:17]2[C:18]3[CH:24]=[CH:23][NH:22][C:19]=3[N:20]=[CH:21][C:16]2=[CH:15][N:14]=1.CC[N:27]([CH:31](C)C)[CH:28]([CH3:30])C.C[C:35]#[N:36]>>[C:13]1([C@@H:8]2[C@H:7]([CH3:6])[CH2:12][CH2:11][N:10]([C:1]([NH:2][C:35]3[CH:30]=[CH:28][N:27]=[CH:31][N:36]=3)=[O:4])[CH2:9]2)[N:17]2[C:18]3[CH:24]=[CH:23][NH:22][C:19]=3[N:20]=[CH:21][C:16]2=[CH:15][N:14]=1
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Komponenten

5

Edukt 4

HCID 276CarbamateHCID 6342Acetonitrile2×HCID 81531DiisopropylethylamineHCID 672171491-((3R,4R)-4-methylpiperidin-3-yl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine hydrochloride

Produkt 1

HCID 67999614(3R,4R)-3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methyl-N-(pyrimidin-4-yl)piperidine-1-carboxamideAusbeute 9 %

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

To solution of 4-aminopyrimidine (0.04 g, 0.43 mmol), TEA (0.07 mL, 0.47 mmol) and DMAP (0.006 g, 0.05 mmol), in MeCN (1 mL) at about 0° C. was added phenyl chloroformate (0.05 mL, 0.41 mmol). The reaction mixture was warmed to ambient temperature and stirred for about 3 h. To the reaction mixture was added water (2 mL) and Et2O (5 mL). The organic layer was separated, washed with water (2 mL), dried over anhydrous MgSO4, filtered, and concd under reduced pressure to provide the crude carbamate. The carbamate was dissolved in MeCN (1 mL) and to it was added a solution of 1-((3R,4R)-4-methylpiperidin-3-yl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine hydrochloride (0.06 g, 0.21 mmol, Example #5 Step J) and DIEA (0.04 mL, 0.21 mmol) in MeCN (1 mL). The reaction mixture was heated to about 70° C. for about 2 h. The solvent was removed under reduced pressure. The crude residue was dissolved in DCM (5 mL) and washed with water (2 mL), brine (3 mL), dried over anhydrous MgSO4, filtered, and concd under reduced pressure. The crude material was purified by RP-HPLC (Table 1, Method e) to give (3R,4R)-3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methyl-N-(pyrimidin-4-yl)piperidine-1-carboxamide (0.007 g, 9%): LC/MS (Table 1, Method b) Rt=1.40 min; MS m/z 377 (M+H)+.

Aufarbeitung

  1. customThe solvent was removed under reduced pressure
  2. dissolutionThe crude residue was dissolved in DCM (5 mL)
  3. washwashed with water (2 mL), brine (3 mL)
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. customThe crude material was purified by RP-HPLC (Table 1, Method e)

Quellen und Nachweise

ORD-Eintrag
ord-2a68e081ac8d4703bec0577e598b2d6d
Quelldatensatz
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08426411B2

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