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Pivalaldehyde → 1-(2-Nitrophenyl)-2,2-dimethyl-1-propanol

HRID 333469
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HRID 333469 반응식
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.[CH3:19][C:20]([CH3:24])([CH3:23])[CH:21]=[O:22]>C1COCC1>[N+:8]([C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[CH:21]([OH:22])[C:20]([CH3:24])([CH3:23])[CH3:19])([O-:10])=[O:9]
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참가 물질

5

반응물 3

HCID 12417PivalaldehydeHCID 69115o-IodonitrobenzeneHCID 178478979HCID 178478979, 화합물

생성물 1

HCID 591895461-(2-Nitrophenyl)-2,2-dimethyl-1-propanol수율 72.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
40 °C

실험 절차

Under a nitrogen atmosphere, a solution of 1-iodo-2-nitrobenzene (3.0 g, 12 mmol) in anhydrous THF (30 mL) was cooled to minus 40° C., and then phenylmagnesium chloride (2 M in THF, 7.2 mL, 14.5 mmol) was added dropwise at a rate that the temperature would not exceed minus 35° C. After the mixture was stirred for 20 minutes at minus 40° C., trimethylacetaldehyde (1.85 mL, 16.8 mmol) was added dropwise and the mixture was stirred for another 30 minutes at minus 40° C. The mixture was gradually warmed up to room temperature, quenched with saturated ammonium chloride (60 mL), poured into water (60 mL), and extracted with ethyl acetate three times (60 mL each). The combined organic phase was dried over Na2SO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography to yield (RS)-1-(2-nitrophenyl)-2,2-dimethyl-1-propanol (1.82 g, 72%) as a yellow solid. 1H NMR (400 MHz, CDCl3): δ 7.82 (d, 1H, J=6.4 Hz, Ph-H), 7.76 (d, 1H, J=6.4 Hz, Ph-H), 7.61 (t, 1H, J=6.4 Hz, Ph-H), 7.39 (t, 1H, J=6.4 Hz, Ph-H), 5.39 (d, 1H, J=2.8 Hz, Ph-CH), 2.14 (d, 1H, J=3.2 Hz, OH), 0.89 (s, 9H, C(CH3)3).

후처리

  1. customexceed minus 35° C
  2. additionwas added dropwise
  3. temperatureThe mixture was gradually warmed up to room temperature
  4. customquenched with saturated ammonium chloride (60 mL)
  5. additionpoured into water (60 mL)
  6. extractionextracted with ethyl acetate three times (60 mL each)
  7. dry with materialThe combined organic phase was dried over Na2SO4
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-54b2d13290d840ebaccae9995de7fb4b
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08877905B2

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