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Water → ethyl 4-{5-[(1,4-diazabicyclo[2.2.2]oct-2-ylmethyl)amino]pyrazin-2-yl}-2-[(3S,4R)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-1,3-thiazole-5-carboxylate

HRID 655744
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 655744
Cl[C:2]1[N:3]=[CH:4][C:5]([C:8]2[N:9]=[C:10]([N:18]3[CH2:23][CH2:22][C@H:21]([NH:24][C:25]([C:27]4[NH:28][C:29]([CH3:34])=[C:30]([Cl:33])[C:31]=4[Cl:32])=[O:26])[C@H:20]([O:35][CH3:36])[CH2:19]3)[S:11][C:12]=2[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[N:6][CH:7]=1.[N:37]12[CH2:44][CH2:43][N:40]([CH2:41][CH2:42]1)[CH2:39][CH:38]2[CH2:45][NH2:46].C(N(CC)C(C)C)(C)C.O>CN1CCCC1=O>[N:37]12[CH2:44][CH2:43][N:40]([CH2:41][CH2:42]1)[CH2:39][CH:38]2[CH2:45][NH:46][C:2]1[N:3]=[CH:4][C:5]([C:8]2[N:9]=[C:10]([N:18]3[CH2:23][CH2:22][C@@H:21]([NH:24][C:25]([C:27]4[NH:28][C:29]([CH3:34])=[C:30]([Cl:33])[C:31]=4[Cl:32])=[O:26])[C@@H:20]([O:35][CH3:36])[CH2:19]3)[S:11][C:12]=2[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[N:6][CH:7]=1
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Komponenten

6

Edukt 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 158394511,4-Diazabicyclo[2.2.2]octan-2-ylmethanamineHCID 59402528ethyl 4-(5-chloropyrazin-2-yl)-2-[(3R,4S)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-1,3-thiazole-5-carboxylate

Produkt 1

HCID 59402477
ethyl 4-{5-[(1,4-diazabicyclo[2.2.2]oct-2-ylmethyl)amino]pyrazin-2-yl}-2-[(3S,4R)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-1,3-thiazole-5-carboxylate
Ausbeute 20,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

Ethyl 4-(5-chloropyrazin-2-yl)-2-[(3S,4R)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-1,3-thiazole-5-carboxylate (Example 59, 330 mg, 0.57 mmol) was added to a solution of 1-(1,4-diazabicyclo[2.2.2]oct-2-yl)methanamine (EP748807, 407 mg, 2.88 mmol) and N,N-Diisopropylethylamine (0.38 mL, 2.88 mmol) in N-methyl 2-pyrrolidinone (5 mL) and the resulting reaction mixture was stirred for 20 h at 80° C. The reaction mixture was cooled to room temperature, poured into water (40 mL) and extracted with ethyl acetate (3×50 mL). The combined organic layer was washed with brine, dried over anhydrous sodium sulphate and concentrated under reduce pressure to yield crude product which was purified by flash column chromatography over silica gel (0-30% methanol in chloroform) to afford 80 mg (20.5%) of ethyl 4-{5-[(1,4-diazabicyclo[2.2.2]oct-2-ylmethyl)amino]pyrazin-2-yl}-2-[(3S,4R)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-1,3-thiazole-5-carboxylate as an off-white solid.

Aufarbeitung

  1. customthe resulting reaction mixture
  2. temperatureThe reaction mixture was cooled to room temperature
  3. extractionextracted with ethyl acetate (3×50 mL)
  4. washThe combined organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulphate
  6. concentrationconcentrated
  7. customto yield crude product which
  8. customwas purified by flash column chromatography over silica gel (0-30% methanol in chloroform)

Quellen und Nachweise

ORD-Eintrag
ord-f0706e60f5294cd09f0b856cf61afab0
Quelldatensatz
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08071605B2

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