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Potassium Carbonate → 4-(2-Keto-1-benzimidazolinyl)-1-[2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethyl]piperidine

HRID 580045
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HRID 580045 반응식
[O:1]=[C:2]1[N:6]([CH:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[NH:3]1.CS(O[CH2:22][CH2:23][C:24]1[CH:39]=[CH:38][C:27]2[O:28][CH2:29][C:30]3[CH:37]=[CH:36][CH:35]=[CH:34][C:31]=3[C:32](=[O:33])[C:26]=2[CH:25]=1)(=O)=O.C([O-])([O-])=O.[K+].[K+]>C(O)C.CO.C(OCC)(=O)C>[O:1]=[C:2]1[N:6]([CH:7]2[CH2:8][CH2:9][N:10]([CH2:22][CH2:23][C:24]3[CH:39]=[CH:38][C:27]4[O:28][CH2:29][C:30]5[CH:37]=[CH:36][CH:35]=[CH:34][C:31]=5[C:32](=[O:33])[C:26]=4[CH:25]=3)[CH2:11][CH2:12]2)[C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[NH:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 886381,3-Dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-oneHCID 108064742-(6,11-Dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethanol methanesulfonate

생성물 1

HCID 134771164-(2-Keto-1-benzimidazolinyl)-1-[2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethyl]piperidine

시약·촉매·용매 3

HCID 702Ethanol용매
HCID 887Methanol용매
HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 5 g (0.023 m) of 4-(2-keto-1-benzimidazolinyl)piperidine, 7.65 g (0.023 m) of 2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethanol methanesulfonate of Example 1 and 3.17 g (0.023 m) of K2CO3 in 30 ml of absolute ethanol and 60 ml of methanol was refluxed overnight (about 16 hours). The reaction mixture was diluted with 800 ml of ethyl acetate, filtered and evaporated in vacuo. The residue was recrystallized from methanol to give after drying at 100° C. in vacuo, 5.78 g (56%) of 4-(2-keto-1-benzimidazolinyl)-1-[2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethyl]piperidine, m.p. 116°-120° C.

후처리

  1. temperaturewas refluxed overnight (about 16 hours)
  2. filtrationfiltered
  3. customevaporated in vacuo
  4. customThe residue was recrystallized from methanol
  5. customto give
  6. dry with materialafter drying at 100° C. in vacuo, 5.78 g (56%) of 4-(2-keto-1-benzimidazolinyl)-1-[2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethyl]piperidine, m.p. 116°-120° C.

출처 및 근거

ORD 기록
ord-8bc0a1f3a1e5491aaa011bfa6a14f5e8
출처 데이터셋
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04751238

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