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

HRID 731555노트

반응식

HRID 731555 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9a796408c7324664a105b8aedfeab023
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585858B2

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