Sodium Hydroxide → HCID 58777817, 화합물

HRID 2368671노트

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HRID 2368671 반응식
[F:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8](O)([CH3:10])[CH3:9].[OH-].[Na+]>I>[F:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]([CH3:10])[CH3:9]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 131295773-Fluoro-α,α-dimethyl-4-pyridinemethanol

생성물 1

HCID 58777817HCID 58777817, 화합물

시약·촉매·용매 1

HCID 24841Hydrogen iodide용매

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온도
140 °C

실험 절차

2-(3-Fluoro-pyridin-4-yl)-propan-2-ol (from the previous step, 6.40 g, 41.3 mmol) was dissolved in 50 mL of 57% HI aqueous solution. Red phosphorus (4.48 g, 144.0 mmol) was added and the mixture was stirred at 140° C. for 5 hours. The reaction mixture was cooled to room temperature, neutralized with 5N aq NaOH and extracted with ether. The combined organic layers were washed with H2O and brine, then dried over Na2SO4 and concentrated under vacuum. The title compound was obtained by distillation. Spectroscopic data: 1H-NMR (300 MHz, CDCl3): δ ppm 1.27 (d, J=7.04 Hz, 6 H), 3.25 (hept, J=7.04 Hz, 1 H), 7.21 (dd, J=5.44 Hz, 1 H), 8.33-8.36 (m, 2 H).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionextracted with ether
  3. washThe combined organic layers were washed with H2O and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-f5b8552523584530980b7dac2e6044ce
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703797B2

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