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Hydrochloric Acid → (2S)-2-(4-Bromophenyl)piperazine

HRID 1091376
ノート
印刷プレビュー

反応式

HRID 1091376 の反応式
Cl.[Br:2][C:3]1[CH:8]=[CH:7][C:6]([C@H:9]2[CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH2:11][N:10]2C(OC(C)(C)C)=O)=[CH:5][CH:4]=1>C(OCC)(=O)C.CO>[Br:2][C:3]1[CH:4]=[CH:5][C:6]([C@H:9]2[CH2:14][NH:13][CH2:12][CH2:11][NH:10]2)=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 53628944(S)-2-(4-bromophenyl)-1,4-di(t-butoxycarbonyl)piperazine

生成物 1

HCID 51894714(2S)-2-(4-Bromophenyl)piperazine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Hydrogen chloride in ethyl acetate solution (4N) was added to a solution of di-tert-butyl (2S)-2-(4-bromophenyl)piperazine-1,4-dicarboxylate (10 g, 22.7 mmol) in methanol (50 ml). The mixture was stirred for one hour at room temperature and the solvent was evaporated under reduced pressure to give white solid. The mixture was partitioned between saturated aqueous sodium bicarbonate and chloroform. The organic layer was washed with brine, dried over magnesium sulfate and concentrated in vacuo to afford (2S)-2-(4-bromophenyl)piperazine as white crystals. Benzylbromide (9.7 g, 56.7 mmol) was added to a solution of sodium hydride (60% in oil, 2.0 g, 50 mmol) and (2S)-2-(4-bromophenyl)piperazine in tetrahydrofuran (50 ml) at room temperature and the mixture was stirred for one hour. The mixture was partitioned between water and chloroform. The organic layer was washed with brine, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting 5-10% methanol in chloroform to furnish (2S)-1,4-Dibenzyl-2-(4-bromophenyl)piperazine (6.1 g, 64%) as a colorless oil.

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. customto give white solid
  3. customThe mixture was partitioned between saturated aqueous sodium bicarbonate and chloroform
  4. washThe organic layer was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-a4db586f836d4f49bd3164542b156bec
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08129377B2

反応ノート

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