Methanol → 7-Chloro-6-((4-oxocyclohexyl)oxy)isoquinolin-1(2H)-one

HRID 2370289노트

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HRID 2370289 반응식
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8](CC3C=CC(OC)=CC=3)[C:9]2=[O:12])=[CH:4][C:3]=1[O:22][CH:23]1[CH2:32][CH2:31][C:26]2(OCC[O:27]2)[CH2:25][CH2:24]1.CO>C(O)(C(F)(F)F)=O>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][NH:8][C:9]2=[O:12])=[CH:4][C:3]=1[O:22][CH:23]1[CH2:24][CH2:25][C:26](=[O:27])[CH2:31][CH2:32]1

참가 물질

4

반응물 2

HCID 887MethanolHCID 592260607-Chloro-6-(1,4-dioxa-spiro[4.5]dec-8-yloxy)-2-(4-methoxy-benzyl)-2H-isoquinolin-1-one

생성물 1

HCID 598182597-Chloro-6-((4-oxocyclohexyl)oxy)isoquinolin-1(2H)-one수율 40.6%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

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온도
150 °C

실험 절차

800 mg (1.94 mmol) of 7-chloro-6-(1,4-dioxa-spiro[4.5]dec-8-yloxy)-2-(4-methoxy-benzyl)-2H-isoquinolin-1-one (65) were dissolved in 3 mL of TFA and heated in a microwave oven at 150° C. for 3 h. Methanol was added and the reaction mixture was evaporated. The crude product was purified by silica gel chromatography to yield 230 mg of 7-chloro-6-(4-oxo-cyclohexyloxy)-2H-isoquinolin-1-one (67). Rt=1.02 min (Method C). Detected mass: 292.1 (M+H+).

후처리

  1. customthe reaction mixture was evaporated
  2. customThe crude product was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-b793b6966c5a4280b5d8cc268c5ff17f
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710077B2

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