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(3-Amino-phenyl)-carbamic acid benzyl ester → HCID 59138727, 화합물

HRID 970662
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반응식

HRID 970662 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:5]=[CH:6][CH:7]=1>C(O)C>[CH:11]([C:12]1[CH:13]=[N:1][C:2]2[C:7]([CH:17]=1)=[CH:6][CH:5]=[C:4]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)[CH:3]=2)=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 12941491(3-Amino-phenyl)-carbamic acid benzyl ester

생성물 1

HCID 59138727HCID 59138727, 화합물수율 197.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A slurry of benzyl 3-aminophenylcarbamate (8.0 g, 0.033 mol) and 2-dimethylaminomethylene-1,3-bis(dimethylimmonio)propane bis(tetrafluoroborate) (31 g, 0.087 mol) in ethanol (400 mL) was heated at reflux for 24 h. The solution was concentrated under vacuum and the residue was dissolved in THF (200 mL) and 1N HCl (200 mL). The reation mixture was stirred at rt overnight, then poured into a saturated solution of sodium bicarbonate (200 mL), and extracted with EtOAc (2×). The combined organic layers were washed with brine, dried (Na2SO4), and concentrated under vacuum to afford the desired product (10.0 g, 99%) as a yellow solid. LC-MS: 2.84 min, 307.1 (M+1).

후처리

  • temperatureat reflux for 24 h
  • concentrationThe solution was concentrated under vacuum
  • dissolutionthe residue was dissolved in THF (200 mL)
  • additionpoured into a saturated solution of sodium bicarbonate (200 mL)
  • extractionextracted with EtOAc (2×)
  • washThe combined organic layers were washed with brine
  • dry with materialdried (Na2SO4)
  • concentrationconcentrated under vacuum
  • 출처 및 근거

    ORD 기록
    ord-9ce9ef2000d04ad293728e0a9a058d8c
    출처 데이터셋
    uspto-grants-2007_12
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07312233B2

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