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Trifluoroacetic acid → HCID 66713692, compound

HRID 1797923
Notes
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Reaction equation

HRID 1797923 reaction equation
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:10]=[CH:11][C:12]3[O:16][C:15](=[O:17])[NH:14][C:13]=3[CH:18]=2)[C:5]([CH3:19])=[CH:4][N:3]=1.Cl.[F:21][C:22]1[C:27]([CH3:28])=[CH:26][C:25]([NH2:29])=[CH:24][C:23]=1[O:30][CH3:31].[C:32]([OH:38])([C:34]([F:37])([F:36])[F:35])=[O:33].ClC1N=CC=CN=1>CC(O)C>[F:35][C:34]([F:37])([F:36])[C:32]([OH:38])=[O:33].[F:21][C:22]1[C:27]([CH3:28])=[CH:26][C:25]([NH:29][C:2]2[N:7]=[C:6]([NH:8][C:9]3[CH:10]=[CH:11][C:12]4[O:16][C:15](=[O:17])[NH:14][C:13]=4[CH:18]=3)[C:5]([CH3:19])=[CH:4][N:3]=2)=[CH:24][C:23]=1[O:30][CH3:31]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 6422Trifluoroacetic acidHCID 744042-ChloropyrimidineHCID 580713875-(2-Chloro-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-oneHCID 667135964-Fluoro-3-methoxy-5-methylanilline hydrochloride

Product 1

HCID 66713692HCID 66713692, compound

Reagents, catalysts & solvents 1

HCID 3776
Isopropanol
Solvent

Conditions

Temperature
77.5 °C

Procedure

Into a three-neck round-bottom flask, 5-(2-chloro-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-one (33.2 g, 120 mmol) and 4-fluoro-3-methoxy-5-methylbenzenamine hydrochloride (32.19 g, 168 mmol) were added, followed by i-PrOH (750 mL) and TFA (23.1 mL, 300 mmol). The reaction mixture was stirred under nitrogen atmosphere with gentle refluxing (note: with overhead stirrer at internal temperature of 75-80° C.). After 22 h, by LC-MS, the reaction was >95% complete (note: when ≦3% of the 2-chloropyrimidine starting material remained, the reaction did not progress much further even after another day or two). The reaction mixture was cooled to room temperature, precipitate was collected by filtration, washing with i-PrOH (˜50 mL×2). Compound 5-(2-(4-fluoro-3-methoxy-5-methylphenylamino)-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-one trifluoroacetate was obtained as a light tan color solid (still a little bit damp) and was added to a NaHCO3 aqueous solution (15.12 g (180 mmol) of NaHCO3 dissolved in 1 L of H2O). The aqueous suspension was stirred at rt overnight. Solid was collected by filtration, washing with H2O (˜150 mL×3), and was further dried under high vacuum. Free base compound 5-(2-(4-fluoro-3-methoxy-5-methylphenylamino)-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-one was obtained as an off-white solid: 44.51 g (93.8% yield).

Workup

  1. waitthe reaction did not progress much further even after another day
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationprecipitate was collected by filtration
  4. washwashing with i-PrOH (˜50 mL×2)

Sources & evidence

ORD record
ord-f599a7c342544afcad6195c6901b112a
Source dataset
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08343954B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes