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

HRID 1361587ノート

反応式

HRID 1361587 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a288a3ca3714433b87346caedd679ce0
出典データセット
uspto-grants-2011_02
特許番号
US07880000B2

反応ノート

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