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

HRID 2080256
Notes
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Reaction equation

HRID 2080256 reaction equation
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
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 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

Product 1

HCID 58388004
6-Amino-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid (5-phenoxy-thiophen-2-ylmethyl)-amide
Yield 18.5%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 57417360Sodium chloride; waterSolvent

Conditions

Temperature
98 °C

Procedure

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.

Workup

  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)

Sources & evidence

ORD record
ord-d38dbe60c48d472faf6e09d792b6defc
Source dataset
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07932272B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes