5-[3-(Bicyclo[2.2.1]hept-2-yloxy)-4-methoxyphenyl]-1,2-dihydro-2-pyrimidinone → HCID 14010190、化合物

HRID 2210488ノート

反応式

HRID 2210488 の反応式
[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH2:3][CH:2]2[O:8][C:9]1[CH:10]=[C:11]([C:17]2[CH:18]=[N:19][C:20](=[O:23])[NH:21][CH:22]=2)[CH:12]=[CH:13][C:14]=1[O:15][CH3:16].[H][H]>C(O)C.[Ni]>[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH2:3][CH:2]2[O:8][C:9]1[CH:10]=[C:11]([C:17]2[CH2:22][NH:21][C:20](=[O:23])[NH:19][CH:18]=2)[CH:12]=[CH:13][C:14]=1[O:15][CH3:16]

参加物

5

反応物 2

HCID 140101785-[3-(Bicyclo[2.2.1]hept-2-yloxy)-4-methoxyphenyl]-1,2-dihydro-2-pyrimidinoneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 14010190HCID 14010190、化合物収率 31.8%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

The pyrimidinone (0.38 g, 1.22 mmol) is dissolved in 20 ml ethanol and treated with 0.5 g, Raney Nickel, 40 psi hydrogen and refluxed for 18 hours. The reaction is cooled, filtered through celite, and the filtrate concentrated in vacuo. The residue is crystallized from ethyl acetate to afford 0.12 g (31.8%) of the dihydro pyrimidinone as a crystalline solid comprising a 7:3 mixture of endo/exo norbornyl isomers.

後処理

  1. temperaturerefluxed for 18 hours
  2. temperatureThe reaction is cooled
  3. filtrationfiltered through celite
  4. concentrationthe filtrate concentrated in vacuo
  5. customThe residue is crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-e4ac5f4b01de4d9a8d6cc32475773d87
出典データセット
uspto-grants-1995_10
特許番号
US05459145

反応ノート

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