Benzyl Bromide → Tert-butyl 4-benzylpiperazine-1-carboxylate

HRID 352776

反応式

HRID 352776 の反応式
[N:1]1([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[CH2:14](Br)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C>C(#N)C>[CH2:14]([N:4]1[CH2:5][CH2:6][N:1]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:2][CH2:3]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylate

生成物 1

HCID 584330Tert-butyl 4-benzylpiperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

In acetonitrile (80 ml), tert-butyl 1-piperazine carboxylate (2.50 g) was dissolved. Under ice cooling, benzyl bromide (1.59 ml) and triethylamine (1.87 ml) were added dropwise to the resulting solution, followed by stirring at room temperature for 90 minutes. After the solvent was distilled off under reduced pressure, distilled water and dichloromethane were added to the residue to separate the organic layer. The organic layer was washed with saturated aqueous NaCl solution and dried over anhydrous sodium sulfate. The residue obtained by distilling off the solvent under reduced pressure was purified by chromatography on a silica gel column (ethyl acetate:hexane=1:20 to 1:5), whereby the title compound (3.12 g, 84%) was obtained as colorless powder.

後処理

  1. distillationAfter the solvent was distilled off under reduced pressure
  2. distillationdistilled water and dichloromethane
  3. additionwere added to the residue
  4. customto separate the organic layer
  5. washThe organic layer was washed with saturated aqueous NaCl solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe residue obtained
  8. distillationby distilling off the solvent under reduced pressure
  9. customwas purified by chromatography on a silica gel column (ethyl acetate:hexane=1:20 to 1:5), whereby the title compound (3.12 g, 84%)
  10. customwas obtained as colorless powder

出典と根拠

ORDレコード
ord-db6b2e86d50d483baa4043eb53a4adb0
出典データセット
uspto-grants-2004_06
特許番号
US06747023B1

関連ノート

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