2-Bromobenzyl bromide → Tert-butyl 4-(2-bromobenzyl)piperazine-1-carboxylate

HRID 731555ノート

反応式

HRID 731555 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.C(N(C(C)C)CC)(C)C.[Br:23][C:24]1[CH:31]=[CH:30][CH:29]=[CH:28][C:25]=1[CH2:26]Br>C(#N)C>[Br:23][C:24]1[CH:31]=[CH:30][CH:29]=[CH:28][C:25]=1[CH2:26][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

参加物

5

反応物 3

HCID 769652-Bromobenzyl bromideHCID 81531DiisopropylethylamineHCID 143452tert-Butyl piperazine-1-carboxylate

生成物 1

HCID 20754660Tert-butyl 4-(2-bromobenzyl)piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of tert-butyl 1-piperazinecarboxylate (5.51 g, 29.623 mmol) in acetonitrile (60 mL) at 0° C. was treated with diisopropylethylamine and 2-bromobenzyl bromide (7.776 g, 31.105 mmol), warmed to room temperature, stirred for 2 hours, and concentrated. The residue was partitioned between ethyl acetate and aqueous NaHCO3. The aqueous layer was extracted with ethyl acetate and the combined extracts were dried (MgSO4), filtered, and concentrated. The concentrate was used directly in the next step without further purification.

後処理

  1. concentrationconcentrated
  2. customThe residue was partitioned between ethyl acetate and aqueous NaHCO3
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. dry with materialthe combined extracts were dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe concentrate was used directly in the next step without further purification

出典と根拠

ORDレコード
ord-9a796408c7324664a105b8aedfeab023
出典データセット
uspto-grants-2009_09
特許番号
US07585858B2

反応ノート

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