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(2R)-4-[5-fluoro-2-(methyloxy)phenyl]-2-hydroxy-4-methyl-2-(trifluoromethyl) pentanoic acid → (2R)-4-[5-Fluoro-2-(methyloxy)phenyl]-4-methyl-2-(trifluoromethyl)-1,2-pentanediol

HRID 1925590
ノート
印刷プレビュー

反応式

HRID 1925590 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]1[CH:9]=[CH:10][C:11]([O:27][CH3:28])=[C:12]([C:14]([CH3:26])([CH3:25])[CH2:15][C@:16]([OH:24])([C:20]([F:23])([F:22])[F:21])[C:17](O)=[O:18])[CH:13]=1>O1CCCC1>[F:7][C:8]1[CH:9]=[CH:10][C:11]([O:27][CH3:28])=[C:12]([C:14]([CH3:26])([CH3:25])[CH2:15][C@@:16]([C:20]([F:22])([F:23])[F:21])([OH:24])[CH2:17][OH:18])[CH:13]=1
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

4

反応物 2

HCID 15965863(2R)-4-[5-fluoro-2-(methyloxy)phenyl]-2-hydroxy-4-methyl-2-(trifluoromethyl) pentanoic acidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 15965864(2R)-4-[5-Fluoro-2-(methyloxy)phenyl]-4-methyl-2-(trifluoromethyl)-1,2-pentanediol収率 44.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

A solution of lithium aluminium hydride (1M in tetrahydrofuran, 12.6 mL, 12.6 mmol) was introduced into a flask under a nitrogen atmosphere. The solution was heated to 50° C. under nitrogen. (2R)-4-[5-fluoro-2-(methyloxy)phenyl]-2-hydroxy-4-methyl-2-(trifluoromethyl) pentanoic acid (2 g, 6.17 mmol) in tetrahydrofuran (4 mL) was then added dropwise using a syringe pump (50 mL/h addition rate). The solution was then stirred for 13 h at 50° C. The reaction mixture was then cooled to 0° C. and quenched with a slow addition (10 mL/h addition rate) of water (0.5 mL) keeping the temperature below 5° C. Once gas evolution stopped, the cloudy solution was allowed to warm to 20° C. and 15% aqueous sodium hydroxide solution (0.5 mL) followed by water (1.5 mL) were added dropwise (40 mL/h addition rate). The slurry was stirred for 15 min at room temperature, filtered and the inorganic salts were washed twice with ethyl acetate (2×10 mL). The organic liquors were then washed successively with 7.5% aqueous sodium bicarbonate solution (20 mL) and saturated brine (20 mL). The organic liquor was split into two equal amounts, the first half was concentrated to dryness to afford the title compound (851 mg) and the second half was re-crystallised from methyl-cyclohexane to afford the title compound (595 mg).

後処理

  1. additionpump (50 mL/h addition rate)
  2. temperatureThe reaction mixture was then cooled to 0° C.
  3. customquenched with a slow addition (10 mL/h addition rate) of water (0.5 mL)
  4. customthe temperature below 5° C
  5. temperatureto warm to 20° C.
  6. additionwere added dropwise
  7. addition(40 mL/h addition rate)
  8. stirringThe slurry was stirred for 15 min at room temperature
  9. filtrationfiltered
  10. washthe inorganic salts were washed twice with ethyl acetate (2×10 mL)
  11. washThe organic liquors were then washed successively with 7.5% aqueous sodium bicarbonate solution (20 mL) and saturated brine (20 mL)
  12. customThe organic liquor was split into two equal amounts
  13. concentrationthe first half was concentrated to dryness

出典と根拠

ORDレコード
ord-6ab3804e9c2f437cb3f44c0ffd36d2c7
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08178573B2

反応ノート

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