Phosphorus oxychloride → 1-Chloro-6-methoxyisoquinoline

HRID 719838노트

반응식

HRID 719838 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[NH:8][CH:7]=[CH:6]2.O=P(Cl)(Cl)[Cl:16]>>[Cl:16][C:9]1[C:10]2[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH:6]=[CH:7][N:8]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 218898546-methoxyisoquinolin-1(2H)-one

생성물 1

HCID 219010741-Chloro-6-methoxyisoquinoline

실험 절차

6-Methoxy-2H-isoquinolin-1-one in POCl3 was heated to gentle reflux for 3 h then evaporated in vacuo. The residue was poured into ice-water (20 mL) and neutralized to pH 10 with 10 M NaOH. Extracted with CHCl3. The organic layer was washed with brine, dried over MgSO4, filtered, evaporated. The residue was purified by flash chromatography (hexane-EtOAc) to afford a white solid.

후처리

  1. temperatureto gentle reflux for 3 h
  2. customthen evaporated in vacuo
  3. additionThe residue was poured into ice-water (20 mL)
  4. extractionExtracted with CHCl3
  5. washThe organic layer was washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was purified by flash chromatography (hexane-EtOAc)
  10. customto afford a white solid

출처 및 근거

ORD 기록
ord-731a4ab402a44243ba25b206546e7f7b
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07132504B2

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