Sodium Hydroxide → HCID 58777817、化合物

HRID 1892245ノート

反応式

HRID 1892245 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 58777817HCID 58777817、化合物

試薬・触媒・溶媒 1

HCID 24841Hydrogen iodide溶媒

反応条件

温度
140 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b6c796d65da344c69d5ceff685730ce5
出典データセット
uspto-grants-2013_08
特許番号
US08507682B2

反応ノート

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