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Triethylamine → 6-Amino-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid (5-phenoxy-thiophen-2-ylmethyl)-amide

HRID 2080256
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2080256
C(O[C:4]([C:6]1[CH:7]=[C:8]2[CH:15]=[CH:14][NH:13][C:9]2=[N:10][C:11]=1[NH2:12])=[O:5])C.[OH-].[Na+].C(N(CC)CC)C.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.[O:52]([C:59]1[S:63][C:62]([CH2:64][NH2:65])=[CH:61][CH:60]=1)[C:53]1[CH:58]=[CH:57][CH:56]=[CH:55][CH:54]=1>C(O)C.[Cl-].[Na+].O>[O:52]([C:59]1[S:63][C:62]([CH2:64][NH:65][C:4]([C:6]2[CH:7]=[C:8]3[CH:15]=[CH:14][NH:13][C:9]3=[N:10][C:11]=2[NH2:12])=[O:5])=[CH:61][CH:60]=1)[C:53]1[CH:54]=[CH:55][CH:56]=[CH:57][CH:58]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 23130515C-(5-Phenoxy thiophen-2-yl)methylamineHCID 58387889Ethyl 6-amino-1H-pyrrolo[2,3-B]pyridine-5-carboxylate

Produkt 1

HCID 58388004
6-Amino-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid (5-phenoxy-thiophen-2-ylmethyl)-amide
Ausbeute 18,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Reaktionsbedingungen

Temperatur
98 °C

Versuchsvorschrift

To a solution of 6-amino-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid ethyl ester described in Preparation Example R-2 (95 mg, 0.46 mmol) in ethanol (10 mL) was added an aqueous solution of 1N sodium hydroxide (5 mL, 5 mmol), which was then heated for 3 hours in an oil bath at 98° C. After cooling the reaction solution, the reaction solution was concentrated until it reached ⅓ of its volume, neutralized with 1N hydrochloric acid, and further concentrated. The resulting crude product was suspended in N,N-dimethylformamide (5 mL), triethylamine (0.096 mL, 0.69 mmol), benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (153 mg, 0.35 mmol) and C-(5-phenoxy-thiophen-2-yl)-methylamine described in Preparation Example 26 (71 mg, 0.35 mmol) were added thereto, followed by stirring at room temperature for 15 hours. After the reaction was completed, the reaction solution was poured into brine, and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, then concentrated, the obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=2:1), and the title compound (31 mg, 0.085 mmol, 18.5%) was obtained.

Aufarbeitung

  1. temperatureAfter cooling the reaction solution
  2. concentrationthe reaction solution was concentrated until it
  3. concentrationfurther concentrated
  4. additionwere added
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated
  8. customthe obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=2:1)

Quellen und Nachweise

ORD-Eintrag
ord-d38dbe60c48d472faf6e09d792b6defc
Quelldatensatz
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07932272B2

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