Triethylamine → N-ethoxycarbonyl-m-bromophenethylamine

HRID 257044노트

반응식

HRID 257044 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[CH2:5][CH2:6][NH2:7].CCN(CC)CC.Cl[C:19]([O:21][CH2:22][CH3:23])=[O:20]>C(Cl)Cl>[CH2:22]([O:21][C:19]([NH:7][CH2:6][CH2:5][C:4]1[CH:8]=[CH:9][CH:10]=[C:2]([Br:1])[CH:3]=1)=[O:20])[CH3:23]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 70217363-Bromophenethylamine

생성물 1

HCID 18963948N-ethoxycarbonyl-m-bromophenethylamine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of m-bromophenethylamine (6.71 g, 33.55 mmol) and Et3N (7 mL, 50.32 mmoL) in CH2Cl2 (100 mL) is cooled to 0° and ethyl chloroformate (4 mL, 50.32 mmoL) is added. After addition is complete the resulting mixture is allowed to come to room temperature and the solvent is removed in vacuo. The residue is then dissolved in EtOAc (200 mL) and the organic phase washed with 2N HCl (1×250 mL), H2O (1×200 mL), saturated NaHCO3 solution (1×200 mL), saturated NaCl solution (1×200 mL), dried over MgSO4 and concentrated in vacuo to give N-ethoxycarbonyl-m-bromophenethylamine.

후처리

  1. additionAfter addition
  2. customto come to room temperature
  3. customthe solvent is removed in vacuo
  4. dissolutionThe residue is then dissolved in EtOAc (200 mL)
  5. washthe organic phase washed with 2N HCl (1×250 mL), H2O (1×200 mL), saturated NaHCO3 solution (1×200 mL), saturated NaCl solution (1×200 mL)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ee8701aded72479ca304cde5cd352229
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05260316

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