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Diethyl Ether → 3-[3-(5-Isopropyl-2,6-dimethoxy-pyrimidine-4-carbonyl)-5-methyl-phenyl]-acrylonitrile

HRID 426182
ノート
印刷プレビュー

反応式

HRID 426182 の反応式
Br[C:2]1[CH:3]=[C:4]([C:9]([C:11]2[C:16]([CH:17]([CH3:19])[CH3:18])=[C:15]([O:20][CH3:21])[N:14]=[C:13]([O:22][CH3:23])[N:12]=2)=[O:10])[CH:5]=[C:6]([CH3:8])[CH:7]=1.C([O-])(=O)C.[Na+].[C:29](#[N:32])[CH:30]=[CH2:31].CCOCC>CN(C=O)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CC(=O)OCC>[CH:17]([C:16]1[C:11]([C:9]([C:4]2[CH:3]=[C:2]([CH:31]=[CH:30][C:29]#[N:32])[CH:7]=[C:6]([CH3:8])[CH:5]=2)=[O:10])=[N:12][C:13]([O:22][CH3:23])=[N:14][C:15]=1[O:20][CH3:21])([CH3:19])[CH3:18]
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

9

反応物 4

HCID 3283Diethyl EtherHCID 7855AcrylonitrileHCID 517045Sodium AcetateHCID 59686860(3-Bromo-5-methyl-phenyl)-(5-isopropyl-2,6-dimethoxy-pyrimidin-4-yl)-methanone

生成物 1

HCID 667055443-[3-(5-Isopropyl-2,6-dimethoxy-pyrimidine-4-carbonyl)-5-methyl-phenyl]-acrylonitrile収率 17%

試薬・触媒・溶媒 4

HCID 167845
palladium(II) acetate
触媒
HCID 178418397HCID 178418397、化合物触媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
111 °C

実験手順

To a stirred solution of (3-bromo-5-methyl-phenyl)-(5-isopropyl-2,6-dimethoxy-pyrimidin-4-yl)-methanone (3.79 g, 10 mmol) in anhydrous DMF (10 ml), was added sodium acetate (902 mg, 1 mmol), palladium acetate (224 mg, 1 mmol), tetrakis(triphenylphosphine)palladium(0) (1.049 g, 4 mmol), and acrylonitrile in this order. The mixture was then stirred at 90-132° C. (oil bath) for ca. 23 hr. After cooling to room temperature, ether and EA (2:1) was added to the reaction mixture. The mixture was then washed with aqueous saturated sodium bicarbonate solution, washed with water twice, dried with anhydrous magnesium sulfate, filtered, and evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent, EA:hexanes (1:4)) to afford 595 mg (17%) of a white solid. Z-isomer (275 mg, 8%) was also obtained as a white solid. m.p. 144-145° C.; 1H NMR (300 MHz, CDCl3) δ 1.19 (6H, d, J=6.9 Hz), 2.42 (3H, s), 2.83 (1H, m), 3.94 (3H, s), 4.08 (3H, s), 5.92 (1H, d, J=16.8 Hz), 7.39 (1H, d, J=16.8 Hz), 7.49 (1H, s), 7.69 (1H, s), 7.75 (1H, s). Z isomer: 1H NMR (300 MHz, CDCl3) δ 1.19 (6H, d, J=7.2 Hz), 2.45 (3H, s), 2.84 (1H, m), 3.93 (3H, s), 4.06 (3H, s), 5.49 (1H, d, J=12.0 Hz), 7.11 (1H, d, J=12.0 Hz), 7.75 (1H, s), 7.90 (1H, s), 7.97 (1H, s).

後処理

  1. temperatureAfter cooling to room temperature
  2. washThe mixture was then washed with aqueous saturated sodium bicarbonate solution
  3. washwashed with water twice
  4. dry with materialdried with anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customThe residue was purified by silica gel column chromatography (eluent, EA:hexanes (1:4))

出典と根拠

ORDレコード
ord-6518990ae20145da851be62dfed149d5
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08106064B2

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