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Trifluoroacetic acid → 4-Aminoisoquinoline-1-carbonitrile

HRID 966916
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HRID 966916 반응식
COC1C=C(OC)C=CC=1C[NH:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([C:17]#[N:18])=[N:9][CH:8]=1.FC(F)(F)C(O)=O>>[NH2:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([C:17]#[N:18])=[N:9][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 218754144-(2,4-Dimethoxy-benzylamino)-isoquinoline-1-carbonitrile

생성물 1

HCID 218752724-Aminoisoquinoline-1-carbonitrile수율 92%

실험 절차

Compound 470C (50 mg, 0.16 mmol) was treated with trifluoroacetic acid (0.5 mL) for 1 h. The highly colored mixture was partitioned between ethyl acetate (30 mL) and 1N NaOH (30 mL). After washing with brine (15 mL), the organic layer was dried over magnesium sulfate and concentrated in vacuo to afford 24 mg (92%) of compound 470D as a yellow solid. HPLC: 99% at 1.09 min (retention time) (Phenomenex C-18, 5 micron column, 4.6×30 mm, eluting with 10-90% aqueous methanol over 2 min containing 0.1% TFA, 4 mL/min, monitoring at 254 nm). MS (ES+): m/z 170.2 [M+H]+.

후처리

  1. customThe highly colored mixture was partitioned between ethyl acetate (30 mL) and 1N NaOH (30 mL)
  2. wash
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
After washing with brine (15 mL)
  • dry with materialthe organic layer was dried over magnesium sulfate
  • concentrationconcentrated in vacuo
  • 출처 및 근거

    ORD 기록
    ord-124328f5d1014e3cac462c6cf1639773
    출처 데이터셋
    uspto-grants-2005_10
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06953679B2

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