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Phosgene → 4-{4-[(2-Phenyl-5-trifluoromethyl-oxazole-4-carbonyl)-amino]-phenyl}-piperazine-1-carboxylic acid (3-methyl-pyridin-2-yl)-amide

HRID 1641845
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Reaktionsgleichung

Reaktionsgleichung von HRID 1641845
[NH2:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N:3]=1.C(N(CC)CC)C.[C:16](Cl)(Cl)=[O:17].C1COCC1.Cl.[N:26]1([C:32]2[CH:37]=[CH:36][C:35]([NH:38][C:39]([C:41]3[N:42]=[C:43]([C:50]4[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=4)[O:44][C:45]=3[C:46]([F:49])([F:48])[F:47])=[O:40])=[CH:34][CH:33]=2)[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1>C(Cl)Cl.CN1CCCC1=O.C(OCC)(=O)C>[CH3:8][C:7]1[C:2]([NH:1][C:16]([N:29]2[CH2:30][CH2:31][N:26]([C:32]3[CH:37]=[CH:36][C:35]([NH:38][C:39]([C:41]4[N:42]=[C:43]([C:50]5[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=5)[O:44][C:45]=4[C:46]([F:47])([F:49])[F:48])=[O:40])=[CH:34][CH:33]=3)[CH2:27][CH2:28]2)=[O:17])=[N:3][CH:4]=[CH:5][CH:6]=1
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Komponenten

9

Edukt 5

HCID 6371PhosgeneHCID 8028TetrahydrofuranHCID 8471Triethylamine2×HCID 153472-Amino-3-methylpyridineHCID 667383362-Phenyl-5-trifluoromethyl-oxazole-4-carboxylic acid (4-piperazin-1-yl-phenyl)-amide hydrochloride

Produkt 1

HCID 57652030
4-{4-[(2-Phenyl-5-trifluoromethyl-oxazole-4-carbonyl)-amino]-phenyl}-piperazine-1-carboxylic acid (3-methyl-pyridin-2-yl)-amide
Ausbeute 16 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6344DichloromethaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
-40 °C

Versuchsvorschrift

To a solution of 2-amino-3-picoline (26 μL, 0.204 mmol) and triethylamine (63 μL, 0.448 mmol) in 5 mL methylene chloride at −40° C. was slowly added a 20% solution of phosgene in THF (118 μL, 0.224 mmol). The reaction mixture was stirred at −40° C. for 1 hr and then a solution of 2-phenyl-5-trifluoromethyl-oxazole-4-carboxylic acid (4-piperazin-1-yl-phenyl)-amide hydrochloride (100 mg, 0.204 mmol) and triethylamine (57 μl, 0.408 mmol) in 8 ml of 1-methyl-2-pyrrolidinone was slowly added and stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate and washed with saturated sodium bicarbonate solution and water. The organic layer was dried over magnesium sulfate, filtered and evaporated to dryness. The residue was purified by flash chromatography (eluting with ethyl acetate/hexane) to yield 4-{4-[(2-phenyl-5-trifluoromethyl-oxazole-4-carbonyl)-amino]-phenyl}-piperazine-1-carboxylic acid (3-methyl-pyridin-2-yl)-amide (18 mg, 16%). ES-MS calcd for C28H25F3N6O3 (m/e) 550.6, obsd 551.1 (M+H).

Aufarbeitung

  1. stirringstirred at room temperature overnight
  2. washwashed with saturated sodium bicarbonate solution and water
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customThe residue was purified by flash chromatography (eluting with ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-6fd4d8ce48fc4a2baf8ec61bff0856e7
Quelldatensatz
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08115011B2

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