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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
ノート
印刷プレビュー

反応式

HRID 1028106 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 7912DiisopropylamineHCID 67184N-bromobutanimideHCID 2724682Lithium diisopropylamideHCID 67237468HCID 67237468、化合物HCID 178418339Butyllithium

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
-78 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-d4507c258a2c4753aeaa283a58aa8512
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08735417B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート