3,3-Dimethyl-1-[2-(6-(3-pyridyl)hex-5 ynoyl)perhydropyridazinyl] pentane-1,2-dione → 3,3-Dimethyl-1-[2-(6-(3-pyridyl)-hexanoyl)perhydropyridazinyl] pentane-1,2-dione

HRID 851949

反応式

HRID 851949 の反応式
[CH3:1][C:2]([CH3:28])([CH2:26][CH3:27])[C:3](=[O:25])[C:4]([CH:6]1[CH2:11][CH2:10][CH2:9][NH:8][N:7]1[C:12](=[O:24])[CH2:13][CH2:14][CH2:15][C:16]#[C:17][C:18]1[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=1)=[O:5]>CO.O=[Pt]=O>[CH3:1][C:2]([CH3:28])([CH2:26][CH3:27])[C:3](=[O:25])[C:4]([CH:6]1[CH2:11][CH2:10][CH2:9][NH:8][N:7]1[C:12](=[O:24])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][C:18]1[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=1)=[O:5]

参加物

4

反応物 1

HCID 184700723,3-Dimethyl-1-[2-(6-(3-pyridyl)hex-5 ynoyl)perhydropyridazinyl] pentane-1,2-dione

生成物 1

HCID 184700753,3-Dimethyl-1-[2-(6-(3-pyridyl)-hexanoyl)perhydropyridazinyl] pentane-1,2-dione

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 887Methanol溶媒

実験手順

0.1 g PtO2 was added to a solution of 3,3-dimethyl-1-[2-(6-(3-pyridyl)hex-5 ynoyl)perhydropyridazinyl] pentane-1,2-dione (0.3 g, 0.8 mmol) in 20 ml dry MeOH. The mixture was under hydrogenation at room pressure (1 atm) overnight. The product was obtained as clear oil after filtering the catalyst, concentration and purifying on a silica gel (0.125 g, 41%). Rf=0.18 (EtOAc). 1H NMR (CDCl3, 400 MHz): δ 0.89 (t, 3H, J=7.4); 1.24 (s, 6H); 1.38 (m, 2H); 1.66 (m, 10H)i 2.14 (m, 2H); 2.63 (m, 2H); 2.82 (m, 2H); 4.60 (m, 2H); 7.23 (m, 4H). Anal. Calcd. for C22H33N3O3: C, 68.19; H, 8.58; N, 10.84. Found: C, 68.40; H. 8.52; N, 10.62.

後処理

  1. customwas under hydrogenation at room pressure (1 atm) overnight
  2. customThe product was obtained as clear oil
  3. filtrationafter filtering
  4. concentrationthe catalyst, concentration
  5. custompurifying on a silica gel (0.125 g, 41%)

出典と根拠

ORDレコード
ord-c653123278c04365a7675c36d4d17247
出典データセット
uspto-grants-2007_08
特許番号
US07253169B2

関連ノート

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