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Diisopropylamine → N-[3-(2-bromo-1,3-thiazol-5-yl)-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl]-acetamide

HRID 1028106
Notes
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Reaction equation

HRID 1028106 reaction equation
[S:1]1[C:5]([C:6]2[CH:7]=[C:8]([NH:23][C:24](=[O:26])[CH3:25])[CH:9]=[C:10]([NH:12][C:13]3[N:18]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:16]=[CH:15][N:14]=3)[CH:11]=2)=[CH:4][N:3]=[CH:2]1.[Li+].CC([N-]C(C)C)C.[Li]CCCC.C(NC(C)C)(C)C.C1C(=O)N([Br:54])C(=O)C1>C1COCC1>[Br:54][C:2]1[S:1][C:5]([C:6]2[CH:7]=[C:8]([NH:23][C:24](=[O:26])[CH3:25])[CH:9]=[C:10]([NH:12][C:13]3[N:18]=[C:17]([C:19]([F:20])([F:21])[F:22])[CH:16]=[CH:15][N:14]=3)[CH:11]=2)=[CH:4][N:3]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 7912DiisopropylamineHCID 67184N-bromobutanimideHCID 2724682Lithium diisopropylamideHCID 67237468HCID 67237468, compoundHCID 178418339Butyllithium

Product 1

HCID 71075242N-[3-(2-bromo-1,3-thiazol-5-yl)-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl]-acetamide
Yield 48%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent3×

Conditions

Temperature
-78 °C

Procedure

A microwave vial containing N-[3-(1,3-thiazol-5-yl)-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl]acetamide (50 mg, 0.132 mmol) in THF (659 μL) was cooled to −78° C. in a dry ice-acetone bath. To the solution was added a stock solution of LDA prepared from the addition of n-BuLi (3.47 μL, 1.52 M, 0.527 mmol) over diisopropylamine (54.7 mg, 0.540) in THF at −78° C. After stirring the suspension for 20 minutes, a solution of NBS (94 mg, 0.527 mmol) in THF (1 mL) was added. The resulting yellow suspension was stirred at −78° C. for 1 h, after which the bath was removed. Once at room temperature, the reaction was treated with sat. NaHCO3(aq) and the phases were separated. The aqueous was extracted 3 times with ethyl acetate. Organic layers were combined, washed with brine, dried with MgSO4, filtered and concentrated under reduced pressure. The residual solid was purified by flash chromatography to yield N-[3-(2-bromo-1,3-thiazol-5-yl)-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl]-acetamide as a beige powder (29 mg, 0.063 nmol, 48%).

Workup

  1. stirringThe resulting yellow suspension was stirred at −78° C. for 1 h
  2. customafter which the bath was removed
  3. additionOnce at room temperature, the reaction was treated with sat. NaHCO3(aq)
  4. customthe phases were separated
  5. extractionThe aqueous was extracted 3 times with ethyl acetate
  6. washwashed with brine
  7. dry with materialdried with MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe residual solid was purified by flash chromatography

Sources & evidence

ORD record
ord-d4507c258a2c4753aeaa283a58aa8512
Source dataset
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08735417B2

Reaction notes

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