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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
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HRID 1028106 반응식
[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
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참가 물질

7

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
-78 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-d4507c258a2c4753aeaa283a58aa8512
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735417B2

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