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Triethylamine → N-(1H-pyrrolo[3,2-c]pyridin-4-yl)cyclopropanecarboxamide

HRID 2201796
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2201796
NC1C2C=CN(C(OCC3C=CC=CC=3)=O)C=2C=CN=1.C(N(CC)CC)C.C1(C(Cl)=O)CC1.[CH:34]1([C:37]([N:39](C(C2CC2)=O)[C:40]2[C:45]3[CH:46]=[CH:47][N:48](C(OCC4C=CC=CC=4)=O)[C:44]=3[CH:43]=[CH:42][N:41]=2)=[O:38])[CH2:36][CH2:35]1.C1(C(NC2C3C=CN(C(OCC4C=CC=CC=4)=O)C=3C=CN=2)=O)CC1.C(=O)([O-])[O-].[K+].[K+]>O1CCCC1.CO>[NH:48]1[C:44]2[CH:43]=[CH:42][N:41]=[C:40]([NH:39][C:37]([CH:34]3[CH2:35][CH2:36]3)=[O:38])[C:45]=2[CH:46]=[CH:47]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 77637Cyclopropanecarbonyl chlorideHCID 71061834benzyl 4-amino-1H-pyrrolo[3,2-c]pyridine-1-carboxylateHCID 86720628benzyl 4-[bis(cyclopropylcarbonyl)amino]-1H-pyrrolo[3,2-c]pyridine-1-carboxylateHCID 86720629
benzyl 4-[(cyclopropylcarbonyl)amino]-1H-pyrrolo[3,2-c]pyridine-1-carboxylate

Produkt 1

HCID 86720627N-(1H-pyrrolo[3,2-c]pyridin-4-yl)cyclopropanecarboxamideAusbeute 69 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
-10 °C

Versuchsvorschrift

To a stirred solution of benzyl 4-amino-1H-pyrrolo[3,2-c]pyridine-1-carboxylate (1 g, 3.5 mmol) in tetrahydrofuran was added triethylamine (1 mL, 7 mmol). The mixture was cooled to −10° C. and cyclopropanecarbonyl chloride (0.53 mL, 5.3 mmol) was added drop wise. The reaction mixture was stirred at room temperature for 1 hour, followed by concentration under vacuum to remove tetrahydrofuran. The residue was dissolved in ethyl acetate and organic layer was washed with water, dried over anhydrous sodium sulfate and concentrated to give the crude mixture of benzyl 4-[bis(cyclopropylcarbonyl)amino]-1H-pyrrolo[3,2-c]pyridine-1-carboxylate and benzyl 4-[(cyclopropylcarbonyl)amino]-1H-pyrrolo[3,2-c]pyridine-1-carboxylate. The mixture was treated with a saturated potassium carbonate solution in methanol and stirred at room temperature followed by removal of methanol under vacuum at the same temperature. The residue was treated drop wise with saturated aqueous sodium bicarbonate solution and the precipitated solid was filtered, washed with water and dried to yield N-(1H-pyrrolo[3,2-c]pyridin-4-yl)cyclopropanecarboxamide (0.5 g, 69%) as a pale yellow solid.

Aufarbeitung

  1. concentrationfollowed by concentration under vacuum
  2. customto remove tetrahydrofuran
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washorganic layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customto give the crude
  8. stirringstirred at room temperature
  9. customfollowed by removal of methanol under vacuum at the same temperature
  10. additionThe residue was treated drop wise with saturated aqueous sodium bicarbonate solution
  11. filtrationthe precipitated solid was filtered
  12. washwashed with water
  13. customdried

Quellen und Nachweise

ORD-Eintrag
ord-06676d7b52c640cd80990399103feb09
Quelldatensatz
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09364466B2

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