1-Methylpiperazine → 1-Methyl-4-(5-nitro-2-pentafluoroethyl-benzyl)-piperazine

HRID 238460ノート

反応式

HRID 238460 の反応式
Br[CH2:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=1[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14].[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>>[CH3:19][N:20]1[CH2:25][CH2:24][N:23]([CH2:2][C:3]2[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=2[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14])[CH2:22][CH2:21]1

参加物

3

反応物 2

HCID 531671-MethylpiperazineHCID 219593672-Bromomethyl-4-nitro-1-pentafluoroethyl-benzene

生成物 1

HCID 222492671-Methyl-4-(5-nitro-2-pentafluoroethyl-benzyl)-piperazine

実験手順

2-Bromomethyl-4-nitro-1-pentafluoroethyl-benzene (2.6 g) was added to N-methylpiperazine (5 ml) and stirred at RT for 3 h. The mixture was filtered and the filtrate was treated with 1-chlorobutane, extracted with 2N HCl (100 ml). The acidic solution was treated with 5N NaOH (6 ml) then extracted with EtOAc. The organic layer was removed, dried over MgSO4 and concentrated to give the compound as an oil.

後処理

  1. filtrationThe mixture was filtered
  2. additionthe filtrate was treated with 1-chlorobutane
  3. extractionextracted with 2N HCl (100 ml)
  4. additionThe acidic solution was treated with 5N NaOH (6 ml)
  5. extractionthen extracted with EtOAc
  6. customThe organic layer was removed
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-735cf649371245afb38e8578bf47715e
出典データセット
uspto-grants-2014_02
特許番号
US08642624B2

反応ノート

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