Sodium Bicarbonate → 7-Chloro-2-(4-methoxy-benzyl)-6-(4-oxo-cyclohexyloxy)-2H-isoquinolin-1-one

HRID 2370288노트

반응식

HRID 2370288 반응식
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=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.C(=O)(O)[O-].[Na+]>Cl.CC(C)=O>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8]([CH2:13][C:14]3[CH:15]=[CH:16][C:17]([O:20][CH3:21])=[CH:18][CH:19]=3)[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 516892Sodium BicarbonateHCID 592260607-Chloro-6-(1,4-dioxa-spiro[4.5]dec-8-yloxy)-2-(4-methoxy-benzyl)-2H-isoquinolin-1-one

생성물 1

HCID 592260557-Chloro-2-(4-methoxy-benzyl)-6-(4-oxo-cyclohexyloxy)-2H-isoquinolin-1-one수율 69.8%

시약·촉매·용매 1

HCID 19044839Acetone hydrogen chloride용매

실험 절차

1.00 g (2.19 mmol) of 7-chloro-6-(1,4-dioxa-spiro[4.5]dec-8-yloxy)-2-(4-methoxy-benzyl)-2H-isoquinolin-1-one (65) were stirred in 9 ml of 6 N HCl/acetone (1:2) at room temperature. After 2 h the reaction mixture was poured on saturated sodium bicarbonate solution and extracted with dichloromethane. The organic layer was dried with magnesium sulfate and evaporated. The crude product was purified by silica gel chromatography to give 630 mg of the title compound. Rt=1.81 min (Method B). Detected mass: 412.2 (M+H+).

후처리

  1. extractionextracted with dichloromethane
  2. dry with materialThe organic layer was dried with magnesium sulfate
  3. customevaporated
  4. customThe crude product was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-188a816c250a400c9bc06cc3a7b222b4
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710077B2

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