Tetrapropylammonium → 1-(3-Isopropyl-1,2,4-oxadiazol-5-YL)piperidin-4-one

HRID 1409739

반응식

HRID 1409739 반응식
[CH3:1][CH:2]([C:4]1[N:8]=[C:7]([N:9]2[CH2:14][CH2:13][CH:12]([OH:15])[CH2:11][CH2:10]2)[O:6][N:5]=1)[CH3:3].C[N+]1([O-])CCOCC1.C([N+](CCC)(CCC)CCC)CC>ClCCl>[CH3:3][CH:2]([C:4]1[N:8]=[C:7]([N:9]2[CH2:10][CH2:11][C:12](=[O:15])[CH2:13][CH2:14]2)[O:6][N:5]=1)[CH3:1]

참가 물질

5

반응물 3

HCID 9559TetrapropylammoniumHCID 82029Methyl morpholine oxideHCID 218977441-(3-Isopropyl-1,2,4-oxadiazol-5-YL)piperidin-4-OL

생성물 1

HCID 669153481-(3-Isopropyl-1,2,4-oxadiazol-5-YL)piperidin-4-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-[3-(Propan-2-yl)-1,2,4-oxadiazol-5-yl]piperidin-4-ol (0.5 g) is dissolved in dichloromethane (75 mL) and 4 A molecular sieves (4 g) are added followed by N-methylmorpholine-N-oxide (1.52 g) and tetrapropylammonium perrhutenate (0.018 g) and the mixture is stirred at room temperature for 1 h. The reaction is then filtered through celite and the mother liquor washed with water (2×50 mL). The water layers are then combined and back extracted with dichloroemthane (100 mL). The dichloromethane layers are combined, dried over Na2SO4, filtered and concentrated to give the title compound. LC (method 20): tR=1.67 min; Mass spectrum (APCI): m/z=210 [M+H]+.

후처리

  1. addition4 A molecular sieves (4 g) are added
  2. filtrationThe reaction is then filtered through celite
  3. washthe mother liquor washed with water (2×50 mL)
  4. extractionback extracted with dichloroemthane (100 mL)
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-38fbc51127124e7badac6fcceb6e2ec6
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921398B2

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