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Cesium carbonate → (E)-2-(3,3-diethoxyprop-1-enyl)-1-fluoro-3-nitrobenzene

HRID 1621836
ノート
印刷プレビュー

反応式

HRID 1621836 の反応式
[CH2:1]([O:3][CH:4]([O:16][CH2:17][CH3:18])[CH:5]=[CH:6]B1OC(C)(C)C(C)(C)O1)[CH3:2].Br[C:20]1[C:25]([N+:26]([O-:28])=[O:27])=[CH:24][CH:23]=[CH:22][C:21]=1[F:29].C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.O.[Pd+2].ClC1C=C[C-](P(C2C=CC=CC=2)C2C=CC=CC=2)C=1Cl.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2]>[CH2:17]([O:16][CH:4]([O:3][CH2:1][CH3:2])/[CH:5]=[CH:6]/[C:20]1[C:25]([N+:26]([O-:28])=[O:27])=[CH:24][CH:23]=[CH:22][C:21]=1[F:29])[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

7

反応物 3

HCID 10796Cesium carbonateHCID 183734742-Bromo-1-fluoro-3-nitrobenzeneHCID 686781162-(3,3-Diethoxy-1-propen-1-YL)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane

生成物 1

HCID 68514002(E)-2-(3,3-diethoxyprop-1-enyl)-1-fluoro-3-nitrobenzene収率 61%

試薬・触媒・溶媒 3

HCID 178478230HCID 178478230、化合物
触媒
HCID 962Water溶媒2 回
HCID 312751,4-Dioxane溶媒

反応条件

温度
120 °C

実験手順

A glass microwave reaction vessel was charged with 3,3-diethoxy-1-propenylboronic acid pinacol ester (0.154 mL, 0.600 mmol, Frontier Scientific), 2-bromo-1-fluoro-3-nitrobenzene (110 mg, 0.500 mmol, Aldrich), dichloro 1,1′-bis(diphenylphosphino)ferrocene palladium (II) (40.8 mg, 0.050 mmol, Strem) and cesium carbonate (326 mg, 1.00 mmol, Aldrich) in dioxane (3 mL) and water (0.5 mL). The reaction mixture was stirred and heated in an Emrys Optimizer microwave reactor (Personal Chemistry, Biotage AB, Inc., Upssala, Sweden) at 120° C. for 20 min. The reaction mixture was diluted with water (10 mL) and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with saturated NaCl (5 mL) and dried over Na2SO4. The solution was filtered and concentrated in vacuo to give the crude material. The crude product was purified by silica gel chromatography eluting with 10% EtOAc/hexanes to give (E)-2-(3,3-diethoxyprop-1-enyl)-1-fluoro-3-nitrobenzene (82 mg, 0.305 mmol, 60.9% yield). 1H NMR (300 MHz, CDCl3) δ 1.26 (t, J=7.02 Hz, 6H) 3.45-3.81 (m, 4H) 5.09 (d, J=4.09 Hz, 1H) 6.16-6.37 (m, 1H) 6.76 (d, J=17.25 Hz, 1H) 7.29-7.53 (m, 2H) 7.57-7.75 (m, 1H). m/z (ESI, +ve ion) 270 (M+H)+.

後処理

  1. customA glass microwave reaction vessel
  2. extractionextracted with EtOAc (2×20 mL)
  3. washThe combined organic extracts were washed with saturated NaCl (5 mL)
  4. dry with materialdried over Na2SO4
  5. filtrationThe solution was filtered
  6. concentrationconcentrated in vacuo
  7. customto give the crude material
  8. customThe crude product was purified by silica gel chromatography
  9. washeluting with 10% EtOAc/hexanes

出典と根拠

ORDレコード
ord-06d8ca6d1ef94606bd16bf6aa4bffd8c
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772480B2

反応ノート

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