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

HRID 238460노트

반응식

HRID 238460 반응식
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

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-735cf649371245afb38e8578bf47715e
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642624B2

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