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Methyl morpholine oxide → 3-(5,6,7,8,9,10-Hexahydro[1,2,4]triazolo[4,3-a]azocin-3-yl)-3-(2-thienyl)cyclobutanone

HRID 502985
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HRID 502985 반응식
[N:1]1[N:2]=[C:3]([C:12]2([C:17]3[S:18][CH:19]=[CH:20][CH:21]=3)[CH2:15][CH:14]([OH:16])[CH2:13]2)[N:4]2[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][C:5]=12.C[N+]1([O-])CCOCC1>C(Cl)Cl>[N:1]1[N:2]=[C:3]([C:12]2([C:17]3[S:18][CH:19]=[CH:20][CH:21]=3)[CH2:13][C:14](=[O:16])[CH2:15]2)[N:4]2[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][C:5]=12
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참가 물질

4

반응물 2

HCID 82029Methyl morpholine oxideHCID 590064423-(5,6,7,8,9,10-Hexahydro[1,2,4]triazolo[4,3-a]azocin-3-yl)-3-(2-thienyl)cyclobutanol

생성물 1

HCID 684665703-(5,6,7,8,9,10-Hexahydro[1,2,4]triazolo[4,3-a]azocin-3-yl)-3-(2-thienyl)cyclobutanone수율 79.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-(5,6,7,8,9,10-hexahydro[1,2,4]triazolo[4,3-a]azocin-3-yl)-3-(2-thienyl)cyclobutanol (2.73 g) was dissolved in methylene chloride (330 ml) and then tetra-n-propylammonium perruthenate(VII) (316 mg) and NMO (1.58 g) were added thereto, followed by stirring at room temperature for 15 hours. The reaction solution was subjected to evaporation under reduced pressure and the resulting residue was purified by column chromatography (methanol:chloroform=3:97) to obtain 2.16 g of 3-(5,6,7,8,9,10-hexahydro[1,2,4]triazolo[4,3-a]azocin-3-yl)-3-(2-thienyl)cyclobutanone (pale yellow solid).

후처리

  1. customThe reaction solution was subjected to evaporation under reduced pressure
  2. customthe resulting residue was purified by column chromatography (methanol:chloroform=3:97)

출처 및 근거

ORD 기록
ord-be047e288f2448ae9583f8d353aba125
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07776897B2

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