Diethyl Malonate → HCID 66737111, 화합물

HRID 2096121노트

반응식

HRID 2096121 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 66737111HCID 66737111, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-50c3a139f6374b10bab4b5b884e6da04
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450243B2

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