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

HRID 36473노트

반응식

HRID 36473 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 14010190HCID 14010190, 화합물수율 31.8%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-01d4b25a8d8a486183035da567d66e31
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05414127

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