2-((1-(Trifluoromethyl)cyclopropyl)methyl)malonic acid → 3-(1-(Trifluoromethyl)cyclopropyl)propanoic acid
反応式
[F:1][C:2]([F:15])([F:14])[C:3]1([CH2:6][CH:7](C(O)=O)[C:8]([OH:10])=[O:9])[CH2:5][CH2:4]1>N1C=CC=CC=1>[F:1][C:2]([F:14])([F:15])[C:3]1([CH2:6][CH2:7][C:8]([OH:10])=[O:9])[CH2:5][CH2:4]1参加物
3
実験手順
A solution of 2-((1-(trifluoromethyl)cyclopropyl)methyl)malonic acid (1.13 g, 5.00 mmol) in pyridine (25 mL) was heated at 100° C. overnight, cooled to RT and concentrated to dryness. The residue was dissolved in 3N HCl, extracted with DCM (3×) and the combined organics were dried over Na2SO4 and concentrated to dryness to afford 3-(1-(trifluoromethyl)cyclopropyl)propanoic acid (664 mg, 73%). 1H NMR (400 MHz, DMSO-d6): δ 12.18 (s, 1H), 2.32 (t, J=8.0 Hz, 2H), 1.79 (t, J=8.0 Hz, 2H), 0.86 (m, 2H), 0.75 (m, 2H).
後処理
- concentrationconcentrated to dryness
- dissolutionThe residue was dissolved in 3N HCl
- extractionextracted with DCM (3×)
- dry with materialthe combined organics were dried over Na2SO4
- concentrationconcentrated to dryness
出典と根拠
- ORDレコード
- ord-00e58a89e8284c1fb93dbce315da2889
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09382228B2
反応ノート
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