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

HRID 2370288ノート

反応式

HRID 2370288 の反応式
[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

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 592260607-Chloro-6-(1,4-dioxa-spiro[4.5]dec-8-yloxy)-2-(4-methoxy-benzyl)-2H-isoquinolin-1-one

生成物 1

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

試薬・触媒・溶媒 1

HCID 19044839Acetone hydrogen chloride溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-188a816c250a400c9bc06cc3a7b222b4
出典データセット
uspto-grants-2014_04
特許番号
US08710077B2

反応ノート

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