Diethyl Malonate → HCID 66737111、化合物

HRID 2096121ノート

反応式

HRID 2096121 の反応式
[NH2:1][C:2]1[C:7]([CH:8]=O)=[CH:6][C:5]([F:10])=[CH:4][N:3]=1.[C:11](OCC)(=[O:18])[CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14].N1CCCCC1>C(O)C>[F:10][C:5]1[CH:6]=[C:7]2[C:2](=[N:3][CH:4]=1)[NH:1][C:11](=[O:18])[C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:8]2

参加物

5

反応物 3

HCID 7761Diethyl MalonateHCID 8082PiperidineHCID 497615922-Amino-5-fluoro-pyridine-3-carbaldehyde

生成物 1

HCID 66737111HCID 66737111、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-amino-5-fluoropyridine-3-carboxaldehyde (2.80 g), diethyl malonate (6.40 g) and piperidine (0.85 g) in ethanol (50 ml) were heated to reflux with stirring for 18 hours, allowed to cool to ambient temperature then evaporated under reduced pressure. The residual solid obtained was washed with diethyl ether then filtered from solution, and sucked to dryness to give the required product as a pale brown solid, 3.97 g. 1H NMR (CDCl3) δ: ca 11.0 (1H, bs), 9.33 (1H, m), 8.66 (1H, d), 8.42 (1H, s), 7.74 (1H, m), 4.45 (2H, q), 1.44 (3H, t).

後処理

  1. temperaturewere heated
  2. temperatureto reflux
  3. customthen evaporated under reduced pressure
  4. customThe residual solid obtained
  5. washwas washed with diethyl ether
  6. filtrationthen filtered from solution

出典と根拠

ORDレコード
ord-50c3a139f6374b10bab4b5b884e6da04
出典データセット
uspto-grants-2013_05
特許番号
US08450243B2

反応ノート

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