Hydrochloric Acid → 3-AMinoMethyl-6-Methyl-4-propyl-1H-pyridin-2-one hydrochloride

HRID 2208653ノート

反応式

HRID 2208653 の反応式
[CH3:1][C:2]1[NH:7][C:6](=[O:8])[C:5]([C:9]#[N:10])=[C:4]([CH2:11][CH2:12][CH3:13])[CH:3]=1.[ClH:14]>CO.[OH-].[OH-].[Pd+2]>[ClH:14].[NH2:10][CH2:9][C:5]1[C:6](=[O:8])[NH:7][C:2]([CH3:1])=[CH:3][C:4]=1[CH2:11][CH2:12][CH3:13]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 156418016-Methyl-2-oxo-4-propyl-1,2-dihydropyridine-3-carbonitrile

生成物 1

HCID 708741233-AMinoMethyl-6-Methyl-4-propyl-1H-pyridin-2-one hydrochloride収率 60%

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 887Methanol溶媒

実験手順

To a stirred solution of 6-methyl-2-oxo-4-propyl-1,2-dihydropyridine-3-carbonitrile (15.0 g, 85.1 mmol) in methanol (600 mL) and concentrated HCl (15 mL) was added Pd(OH)2 (15.0 g). The mixture was stirred for 48 hours under H2 atmosphere. The reaction mixture was filtered and filtrate was concentrated in vacuo. Ethanol was added to the residue, the resulting precipitate was collected and dried to give the titled compound as a white solid (13.0 g, 60% yield). 1H-NMR (400 MHz, CDCl3) δppm; 11.86 (br. s., 1H), 6.00 (s, 1H), 3.78 (q, J=5.5 Hz, 2H), 3.61 (br. s., 2H), 2.46 (m, 2H), 2.17 (s, 3H), 1.50 (sxt, J=7.4 Hz, 2H), 0.91 (t, J=7.4 Hz, 3H).

後処理

  1. filtrationThe reaction mixture was filtered
  2. concentrationfiltrate was concentrated in vacuo
  3. additionEthanol was added to the residue
  4. customthe resulting precipitate was collected
  5. customdried

出典と根拠

ORDレコード
ord-564a4425e24e45e5ad85d2751ae845a4
出典データセット
uspto-grants-2016_06
特許番号
US09376422B2

反応ノート

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