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Isobutyraldehyde → 2-Methyl-1-(2-nitrophenyl)propan-1-ol

HRID 333462
ノート
印刷プレビュー

反応式

HRID 333462 の反応式
I[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].C1([Mg]Cl)C=CC=CC=1.[CH:19](=[O:23])[CH:20]([CH3:22])[CH3:21]>C1COCC1>[N+:8]([C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[CH:19]([OH:23])[CH:20]([CH3:22])[CH3:21])([O-:10])=[O:9]
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

5

反応物 3

HCID 6561IsobutyraldehydeHCID 69115o-IodonitrobenzeneHCID 178478979HCID 178478979、化合物

生成物 1

HCID 591894222-Methyl-1-(2-nitrophenyl)propan-1-ol収率 99.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

To a solution of 1-iodo-2-nitrobenzene (1.12 g, 4.5 mmol) in anhydrous THF (15 mL) cooled to minus 40° C. under nitrogen atmosphere, a solution of phenylmagnesium chloride (2 M in THF, 2.4 mL, 4.8 mmol) was added dropwise at a rate that the temperature would not exceed minus 35° C. Upon completion of the addition the mixture was stirred for five minutes at minus 40° C., followed by addition of isobutyraldehyde (0.545 mL, 6.0 mmol). The mixture was gradually warmed up to room temperature, quenched with saturated ammonium chloride (6 mL), poured into water (80 mL), and extracted with ethyl acetate three times (100 mL). Combined organic phase was washed with brine (80 mL), dried over Na2SO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography to yield racemic (RS)-1-(2-nitrophenyl)-2-methyl-propanol (0.876 g, 99%) as a light yellow oil. 1H NMR (400 MHz, CDCl3): δ 7.84 (dd, 1H, J=1.2 and 8.2 Hz, Ph-H), 7.73 (dd, 1 H, J=1.4 and 7.9 Hz, Ph-H), 7.61 (m, 1H, Ph-H), 7.39 (m, 1H, Ph-H), 5.03 (dd, 1H, J=4.5 and 5.8 Hz, Ph-CH), 2.42 (d, 1H, J=4.5 Hz, OH), 2.02 (m, 1H, CH), 0.95 (d, 3H, J=6.7 Hz, CH3), 0.89 (d, 3H, J=6.8 Hz, CH3); 13C NMR (100 MHz, CDCl3): δ 148.48 (C), 138.91 (C), 132.95 (CH), 128.85 (CH), 127.95 (CH), 124.21 (CH), 73.79 (CH), 34.30 (CH), 19.66 (CH3), 17.01 (CH3).

後処理

  1. customexceed minus 35° C
  2. additionUpon completion of the addition the mixture
  3. temperatureThe mixture was gradually warmed up to room temperature
  4. customquenched with saturated ammonium chloride (6 mL)
  5. additionpoured into water (80 mL)
  6. extractionextracted with ethyl acetate three times (100 mL)
  7. washCombined organic phase was washed with brine (80 mL)
  8. dry with materialdried over Na2SO4
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-823cf3c74467441ea9fee003892db5ca
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877905B2

反応ノート

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