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Ethylenediamine → HCID 71262272, 화합물

HRID 540350
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HRID 540350 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([N:12]2[CH2:18][C:17]3[CH:19]=[CH:20][CH:21]=[CH:22][C:16]=3[O:15][CH2:14][CH2:13]2)[CH:3]=1.[CH2:23]([NH2:26])[CH2:24][NH2:25]>>[O:15]1[C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[CH2:18][N:12]([C:4]2[CH:3]=[C:2]([NH:25][CH2:24][CH2:23][NH2:26])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[N:5]=2)[CH2:13][CH2:14]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 3301EthylenediamineHCID 71255169HCID 71255169, 화합물

생성물 1

HCID 71262272HCID 71262272, 화합물

반응 조건

온도
150 °C

실험 절차

The mixture of 4-(4-chloroquinolin-2-yl)-2,3,4,5-tetrahydro-1,4-benzoxazepine (100 mg, 0.32 mmol) and 1.6 mL of ethane-1,2-diamine was heated with stirring in a 5 mL microwave process vial for 3 hours at 150° C. under microwave irradiation. The mixture was concentrate in vacuo to give a residue which was purified by preparative HPLC to give 31 mg of product as a white solid. MS obsd. (ESI+) [(M+H)+] 335. 1H NMR (400 MHz, CD3OD) δ ppm 8.61 (s, 1 H), 7.90 (d, J=7.6 Hz, 1 H), 7.60-7.51 (m, 3 H), 7.23 (brs, 2 H), 7.09-6.98 (m, 2 H), 6.05 (s, 1 H), 4.89 (s, 2 H), 4.27 (s, 2 H), 4.25 (s, 2 H), 3.61 (s, 2 H), 3.15 (s, 2 H).

후처리

  1. temperaturewas heated
  2. concentration
The mixture was concentrate in vacuo
  • customto give a residue which
  • customwas purified by preparative HPLC
  • 출처 및 근거

    ORD 기록
    ord-4c2bf6f2ba0644dcafef8a489d6bb9d3
    출처 데이터셋
    uspto-grants-2014_10
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08871756B2

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