1-Methylpiperazine → 1-Methyl-4-[2-nitro-4-(trifluoromethyl)phenyl]piperazine

HRID 1361587노트

반응식

HRID 1361587 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[CH3:15][N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1.C([O-])(O)=O.[Na+]>C1COCC1>[CH3:15][N:16]1[CH2:21][CH2:20][N:19]([C:2]2[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=2[N+:12]([O-:14])=[O:13])[CH2:18][CH2:17]1

참가 물질

5

반응물 3

HCID 531671-MethylpiperazineHCID 677784-Fluoro-3-nitrobenzotrifluorideHCID 516892Sodium Bicarbonate

생성물 1

HCID 28607241-Methyl-4-[2-nitro-4-(trifluoromethyl)phenyl]piperazine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Example 18 was prepared in accordance to a procedure described in Collins, et. al., Tetrahedron, 48, No. 37, pp 7887-7898, 1992. To a solution of 1-Fluoro-2-nitro-4-trifluoromethyl-benzene (1.0 g, 4.78 mmol) in dry THF (24 mL) was added 1-Methyl-piperazine (0.64 mL, 5.74 mmol). The solution turned bright yellow. NaHCO3 (1.1 g, 13 mmol) was added and the reaction was stirred at room temperature and monitored by LCMS: The reaction was filtered and concentrated before being taken up in CH2Cl2 and H2O. The organic layer was separated, dried with MgSO4, filtered, and concentrated to afford the title compound as an orange-brown oil.

후처리

  1. customExample 18 was prepared in accordance to a procedure
  2. filtrationThe reaction was filtered
  3. concentrationconcentrated
  4. customThe organic layer was separated
  5. dry with materialdried with MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a288a3ca3714433b87346caedd679ce0
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07880000B2

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