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Tetrahydrofuran → (2-Cyano-5-(isothiazol-4-ylmethoxy)phenoxy]-4-(2-methylphenyl)butanoic acid

HRID 322916
ノート
印刷プレビュー

反応式

HRID 322916 の反応式
O[C@@H:2]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:14])[CH2:3][CH2:4][C:5]([O-:7])=[O:6].[Na+].[H-].[Na+].F[C:19]1[CH:26]=[C:25]([O:27][CH2:28][C:29]2[CH:30]=[N:31][S:32][CH:33]=2)[CH:24]=[CH:23][C:20]=1[C:21]#[N:22].[O:34]1CCCC1>>[C:21]([C:20]1[CH:23]=[CH:24][C:25]([O:27][CH2:28][C:29]2[CH:30]=[N:31][S:32][CH:33]=2)=[CH:26][C:19]=1[O:34][CH:4]([CH2:3][CH2:2][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:14])[C:5]([OH:7])=[O:6])#[N:22]
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 4

HCID 8028Tetrahydrofuran2 回HCID 24758Sodium hydrideHCID 220102302-Fluoro-4-(isothiazol-4-ylmethoxy)benzonitrileHCID 86756593Sodium (R)-4-Hydroxy-4-(2-methylphenyl)butanoate

生成物 1

HCID 23204063(2-Cyano-5-(isothiazol-4-ylmethoxy)phenoxy]-4-(2-methylphenyl)butanoic acid

反応条件

温度
50 °C

実験手順

Sodium (R)-4-Hydroxy-4-(2-methylphenyl)butanoate (0.39 g) is added in one portion to a stirred suspension of sodium hydride (0.11 g, 60% dispersion in mineral oil) in tetrahydrofuran (30 mL) and the mixture is stirred at 50° C. for 1 hour. A solution of 2-fluoro-4-(isothiazol-4-ylmethoxy)benzonitrile (0.21 g) in tetrahydrofuran (20 mL) is added and the reaction mixture is stirred at reflux for 16 hours. The reaction mixture is concentrated in vacuo and water is added to the residue. The solution is acidified with 1 N hydrochloric acid and extracted with ethyl acetate (50 mL). The organic phase is washed with water (50 mL), with brine (50 mL), dried over magnesium sulphate and evaporated. The residue is purified by flash chromatography on silica eluting with a mixture of dichloromethane and methanol (19:1 v/v). Fractions homogeneous in the required product are combined and evaporated to give (R)-4-[(2-cyano-5-(isothiazol-4-ylmethoxy)phenoxy]-4-(2-methylphenyl)butanoic acid, (0.02 g) in the form of a yellow oil. [NMR (CDCl3) (300 MHz): -2.2-2.4 (m, 2H), 2.45 (s, 3H), 2.6-2.65 (m), 2.75-2.8 (m,1H), 5.0 (q, 2H), 5.5 (dd,1H), 6.15 (d,1H), 6.5 (dd, 1H), 7.2 (m, 3H), 7.4 (m,1H), 7.45 (d,1H), 8.45 (d, 2H)].

後処理

  1. stirringthe reaction mixture is stirred
  2. temperatureat reflux for 16 hours
  3. concentrationThe reaction mixture is concentrated in vacuo and water
  4. additionis added to the residue
  5. extractionextracted with ethyl acetate (50 mL)
  6. washThe organic phase is washed with water (50 mL), with brine (50 mL)
  7. dry with materialdried over magnesium sulphate
  8. customevaporated
  9. customThe residue is purified by flash chromatography on silica eluting with a mixture of dichloromethane and methanol (19:1 v/v)
  10. customevaporated

出典と根拠

ORDレコード
ord-3c1ec38766f64f00a5473449b4cc8d27
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06211234B1

反応ノート

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