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

HRID 2201796
Notes
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Reaction equation

HRID 2201796 reaction equation
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
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

9

Reactant 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

Product 1

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

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 8028TetrahydrofuranSolvent

Conditions

Temperature
-10 °C

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-06676d7b52c640cd80990399103feb09
Source dataset
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09364466B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes