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

반응식

HRID 851949 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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%)

출처 및 근거

ORD 기록
ord-c653123278c04365a7675c36d4d17247
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253169B2

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