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Ethyl Propionate → (S)-2-(2-Oxo-2H-pyrid-1-yl)-propionic acid ethyl ester

HRID 602919
ノート
印刷プレビュー

反応式

HRID 602919 の反応式
[NH:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]1=[O:7].[H-].[Na+].[CH2:10]([O:12][C:13](=[O:16])[CH2:14][CH3:15])[CH3:11]>C1COCC1>[CH2:10]([O:12][C:13](=[O:16])[C@@H:14]([N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]1=[O:7])[CH3:15])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7749Ethyl PropionateHCID 88712-PyridoneHCID 24758Sodium hydride

生成物 1

HCID 66650045(S)-2-(2-Oxo-2H-pyrid-1-yl)-propionic acid ethyl ester収率 46.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A stirred solution of 1H-Pyridin-2-one (500 mg, 5.26 mmol) in anhydrous THF (50 ml) at room temperature was treated portionwise with 60% NaH (231 mg, 5.78 mmol). The reaction mixture was kept for 10 min then added over 5 min to a solution of (R)-2-trifluoromethanesulfonyloxy)-propionic acid ethyl ester (1315 mg, 5.26 mmol) in anhydrous THF (2.5 ml) at room temperature. The resulting mixture was stirred for 2 h, then concentrated. The residue was dissolved in ethyl acetate, and the resulting solution was washed with ice cold dilute HCl. The organic layer was removed and the aqueous layer re-extracted with ethyl acetate. The combined organic extracts were dried (MgSO4), filtered and concentrated. The residue was purified by flash chromatography (20% up to 80% ethyl acetate in hexane) to afford the title compound as a yellow oil (480 mg, 46%): [α]27D=−56.4° (c=0.275, CH2Cl2); 1H NMR (400 MHz CDCl3) δ 1.3 (3H, t), 1.65 (3H, d), 4.2 (2H, q), 5.6 (1H, q), 6.2 (1H, t), 6.4 (1H, d), 7.2-7.3 (2H, m).

後処理

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washthe resulting solution was washed with ice cold dilute HCl
  4. customThe organic layer was removed
  5. extractionthe aqueous layer re-extracted with ethyl acetate
  6. dry with materialThe combined organic extracts were dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified by flash chromatography (20% up to 80% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-ead1519f8bbb4c039e3fd665ac4f08e8
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07906650B2

反応ノート

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