tert-Butyl piperazine-1-carboxylate → 1-Boc-4-(5-nitro-2-pentafluoroethyl-benzyl)-piperazine

HRID 238461ノート

反応式

HRID 238461 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].[C:19]([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20].C([O-])(O)=O.[Na+]>C(Cl)Cl>[C:19]([N:26]1[CH2:27][CH2:28][N:29]([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])[CH2:30][CH2:31]1)([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20]

参加物

5

反応物 3

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 516892Sodium BicarbonateHCID 219593672-Bromomethyl-4-nitro-1-pentafluoroethyl-benzene

生成物 1

HCID 222492271-Boc-4-(5-nitro-2-pentafluoroethyl-benzyl)-piperazine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

2-Bromomethyl-4-nitro-1-pentafluoroethyl-benzene (2.5 g) was dissolved in CH2Cl2 and added to N-Boc-piperazine (2.5 g) and NaHCO3 (1 g) and stirred at RT overnight. The mixture was diluted with CH2Cl2 (100 ml), washed with sat'd NH4Cl, dried over MgSO4, filtered and concentrated. The residue was purified by silica gel chromatography (hexane, CH2Cl2:hexane 2:8) to give the compound as an yellow solid.

後処理

  1. washwashed with sat'd NH4Cl
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel chromatography (hexane, CH2Cl2:hexane 2:8)

出典と根拠

ORDレコード
ord-58649019a85e4bb3bea84c4ffc574e90
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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