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Ethyl(3-methoxy-4-nitrobenzyl)methylphosphinate → HCID 178491642, 화합물

HRID 1948025
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HRID 1948025 반응식
C([P:3]([CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[C:10]([O:17][CH3:18])[CH:9]=1)(=[O:5])[O-:4])C>Cl>[CH3:18][O:17][C:10]1[CH:9]=[C:8]([CH:13]=[CH:12][C:11]=1[N+:14]([O-:16])=[O:15])[CH2:7][CH2:6][PH:3](=[O:4])[OH:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 86654041Ethyl(3-methoxy-4-nitrobenzyl)methylphosphinate2회

생성물 1

HCID 178491642HCID 178491642, 화합물수율 102%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of ethyl(3-methoxy-4-nitrobenzyl)methylphosphinate (Compound 216D, 0.500 g, 1.83 mmol) in 37% HCl (5.00 mL) was stirred at 100° C. for 6 hours. The reaction mixture was concentrated under reduced pressure to yield the desired product as a yellow foam, 457.2 mg (102% yield). This material was used in successive reactions without any further purification. 1H NMR (CDCl3, 400 MHz): δ=1.41 (d, J=13.89 Hz, 3H), 3.13 (d, J=16.42 Hz, 2H), 3.97 (s, 3H), 6.89 (d, J=8.08 Hz, 1H), 7.02 (s, 1H), 7.82 (d, J=8.34 Hz, 1H). MS (ES+): m/z 246.05 [MH+] (TOF, polar).

후처리

  • concentrationThe reaction mixture was concentrated under reduced pressure
  • 출처 및 근거

    ORD 기록
    ord-ac3f8dccfb134e079fb7e8ccba9ea982
    출처 데이터셋
    uspto-grants-2013_03
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08399433B2

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