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Diisopropylethylamine → 4H-Pyrido[1,2-a]pyrimidin-4-one

HRID 405958
Notes
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Reaction equation

HRID 405958 reaction equation
BrC1N=CN=C2C=1NC=N2.NC[C:13]1[N:14]=[C:15]2[CH:30]=[CH:29][CH:28]=[C:27](C)[N:16]2[C:17](=[O:26])[C:18]=1C1C=CC=C(F)C=1.CCN(C(C)C)C(C)C>C(O)CCC>[N:14]1[CH:13]=[CH:18][C:17](=[O:26])[N:16]2[CH:27]=[CH:28][CH:29]=[CH:30][C:15]=12
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 81531DiisopropylethylamineHCID 5287830Purine, 6-bromo-HCID 66831387HCID 66831387, compound

Product 1

HCID 3547854H-Pyrido[1,2-a]pyrimidin-4-one

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Conditions

Temperature
110 °C

Procedure

A mixture of 6-bromopurine (0.02040 g, 0.1025 mmol), 2-(aminomethyl)-3-(3-fluorophenyl)-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (0.02420 g, 0.08542 mmol), and DIEA (0.04464 mL, 0.2563 mmol) in 1-butanol (2.000 mL) was stirred at 110° C. After 18 h, the mixture was removed from the heat and concd under reduced pressure. The crude mixture was purified by revered-phase semi-prep HPLC using 20-70% gradient of CH3CN (0.1% of TFA) in water (0.1% of TFA) over 40 min as eluent. The acetonitrile was concd under reduced pressure and to the remaining acidic aq layer was added satd NaHCO3 to neutralize the TFA salt. The resulting precipitate was collected by filtration and washed with water to give 3-(3-fluorophenyl)-6-methyl-249H-purin-6-ylamino)methyl)-4H-pyrido[1,2-a]pyrimidin-4-one as a light yellow solid: 1H NMR (400 MHz, DMSO-d6) δ ppm 12.87 (1 H, s), 8.07-8.16 (2 H, m), 7.68 (1 H, dd, J=9.0, 7.0 Hz), 7.55 (1 H, s), 7.39-7.51 (2 H, m), 7.24-7.31 (2 H, m), 7.15-7.23 (1 H, m), 6.92-7.00 (1 H, m), 4.51 (2 H, br. s.), 2.92 (3 H, s); Mass Spectrum (ESI) m/e=402.1 (M+1).

Workup

  1. customthe mixture was removed from the
  2. temperatureheat
  3. customThe crude mixture was purified by revered-phase semi-prep HPLC
  4. customover 40 min
  5. additionwas added satd NaHCO3
  6. filtrationThe resulting precipitate was collected by filtration
  7. washwashed with water

Sources & evidence

ORD record
ord-a462b6d650db4109a94b8beab57aa644
Source dataset
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08754089B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes