Phosphorus oxychloride → 1-Chloro-6-methoxy-3-methylisoquinoline

HRID 1511472

반응식

HRID 1511472 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][C:7]([CH3:14])=[CH:6]2.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:9]1[C:10]2[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH:6]=[C:7]([CH3:14])[N:8]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 123270606-Methoxy-3-methylisoquinolin-1(2H)-one

생성물 1

HCID 578930951-Chloro-6-methoxy-3-methylisoquinoline

실험 절차

The isoquinoline of step 2 was dissolved in phosphorus oxychloride (2.5 mL) and heated at reflux for 1 hour. The excess phosphorus oxychloride was removed under reduced pressure and the residue was dissolved in chloroform. The resulting solution was washed with 1N aq. sodium hydroxide, water and brine. Evaporation of the solvent under reduced pressure gave crude 1-chloro-6-methoxy-3-methylisoquinoline, which was used directly in the next step.

후처리

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. customThe excess phosphorus oxychloride was removed under reduced pressure
  4. dissolutionthe residue was dissolved in chloroform
  5. washThe resulting solution was washed with 1N aq. sodium hydroxide, water and brine
  6. customEvaporation of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-04e0c1e65adf462e83c139abb7ab8e91
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08211897B2

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