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Tetrahydrofuran → Ethyl 4-{[2-(methylsulfanyl)pyrimidin-5-yl]methyl}quinoline-2-carboxylate

HRID 1497331
ノート
印刷プレビュー

反応式

HRID 1497331 の反応式
CC1(C)C(C)(C)OB([C:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[N:12]=[C:11]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:10]=2)O1.Br[CH2:26][C:27]1[CH:28]=[N:29][C:30]([S:33][CH3:34])=[N:31][CH:32]=1.C(=O)([O-])[O-].[Cs+].[Cs+].C1COCC1>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl.O>[CH3:34][S:33][C:30]1[N:31]=[CH:32][C:27]([CH2:26][C:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[N:12]=[C:11]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:10]=2)=[CH:28][N:29]=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 4

HCID 8028TetrahydrofuranHCID 10796Cesium carbonateHCID 60209908Ethyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)quinoline-2-carboxylateHCID 60209911HCID 60209911、化合物

生成物 1

HCID 60209912Ethyl 4-{[2-(methylsulfanyl)pyrimidin-5-yl]methyl}quinoline-2-carboxylate

試薬・触媒・溶媒 2

HCID 178418807
HCID 178418807、化合物
触媒
HCID 962Water溶媒

反応条件

温度
77 °C

実験手順

In a microwave vial containing ethyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)quinoline-2-carboxylate (K4) (0.15 g, 0.46 mmol), 5-(bromomethyl)-2-(methylsulfanyl)pyrimidine (N3) (0.12 g, 0.55 mmol), cesium carbonate (0.45 g, 1.4 mmol), and PdCl2(dppf)-CH2Cl2 adduct (0.037 g, 0.05 mmol) was added 4.1 mL THF and 0.41 mL water. The reaction mixture was heated to 77° C. for 1 h. The reaction mixture was cooled to room temperature, quenched with water, extracted with ethyl acetate, washed with brine, dried over sodium sulfate, filtered, and concentrated. The resultant residue was subjected to silica gel chromatography eluting with 0-70% ethyl acetate in hexanes to afford ethyl 4-{[2-(methylsulfanyl)pyrimidin-5-yl]methyl}quinoline-2-carboxylate (N4) that gave a mass ion (ES+) of 340.3 for M+H+. The above compound was converted to the titled compound by the procedure described in Example 11 that gave proton NMR spectra consistent with theory and a mass ion (ES+) of 411.1481 for M+H30 . 1H NMR (400 MHz, CDCl3) δ 8.42 (s, 2H), 8.37 (d, J=6.4 Hz, 1H), 8.19 (d, J=8.2 Hz, 1H), 8.14 (s, 1H), 7.99 (d, J=8.4 Hz, 1H), 7.84-7.80 (m, 1H), 7.70-7.66 (m, 1H), 4.44 (s, 2H), 4.13 (dd, J=4.9, 11.2 Hz, 1H), 4.08-4.00 (m, 2H), 3.77-3.71 (m, 1H), 3.55-3.49 (m, 1H), 3.30-3.25 (m, 1H), 2.54 (s, 3H), 2.15-2.11 (m, 1H) 1.95-1.85 (m, 1H).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customquenched with water
  3. extractionextracted with ethyl acetate
  4. washwashed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. washeluting with 0-70% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-152cef85e598459bb67cfe31177e127f
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09199939B2

反応ノート

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