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Ethylenediamine → N,N-Bis-Carbobenzyloxyethylenediamine

HRID 1883298
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HRID 1883298 반응식
Cl[C:2]([O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:3].[CH2:12]([NH2:15])[CH2:13][NH2:14].[OH-:16].[Na+]>>[C:2]([N:14]([C:2]([O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:16])[CH2:13][CH2:12][NH2:15])([O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 3301EthylenediamineHCID 10387Benzyl chloroformateHCID 14798Sodium Hydroxide

생성물 1

HCID 23510767N,N-Bis-Carbobenzyloxyethylenediamine

실험 절차

Benzyl chloroformate (40 mL, 280 mmol) was added dropwise over 45 min to a vigorously stirred solution of ethylenediamine (9.4 mL, 0.5 equiv) in 1M NaOH (310 mL, 1 equiv) at 0° C. A heavy white precipitate formed and the mixture was stirred for 4 h following addition. The resulting solid product was collected by filtration, washed with water and then hexane, and then air-dried overnight (46.17 g, 100%). 1H-NMR (CDCl3) δ 3.32 (s, 4H), 5.10 (s, 4H), 5.23 (br, 2H), 7.35 (s, 10HS MS (ESI) 329.3 (MH)+.

후처리

  1. customA heavy white precipitate formed
addition
addition
  • filtrationThe resulting solid product was collected by filtration
  • washwashed with water
  • dry with materialhexane, and then air-dried overnight (46.17 g, 100%)
  • 출처 및 근거

    ORD 기록
    ord-a2a0237d920f4601b0a28b2c68e5d757
    출처 데이터셋
    uspto-grants-2004_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06759509B1

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