Cesium carbonate → 6-Fluoro-2-[(4-methoxyphenyl)methyl]isoquinolin-1-one

HRID 1930204

反応式

HRID 1930204 の反応式
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7]Cl)=[CH:5][CH:4]=1.[F:11][C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][CH:21]=1)[C:18](=[O:22])[NH:17][CH:16]=[CH:15]2.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C>[F:11][C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][CH:21]=1)[C:18](=[O:22])[N:17]([CH2:7][C:6]1[CH:9]=[CH:10][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)[CH:16]=[CH:15]2

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 699934-Methyloxybenzyl chlorideHCID 450908026-Fluoroisoquinolin-1(2H)-one

生成物 1

HCID 598182606-Fluoro-2-[(4-methoxyphenyl)methyl]isoquinolin-1-one収率 93.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

169 μL of p-methoxybenzylchloride (1.24 mmol, 1.1 eq) were added to a suspension of 200 mg of 6-fluoro-isoquinolinone (13) (1.13 mmol) and 368 mg of Cs2CO3 (1.36 mmol, 1.2 eq) in 3 mL of DMF. The mixture was stirred for 2 h and then poured on ice. The precipitate was filtered, washed with water and dried to yield 300 mg of the title compound. LCMS Method B, retention time 1.76 min, detected mass 284.14 [M+H]+

後処理

  1. additionpoured on ice
  2. filtrationThe precipitate was filtered
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-69a7ed0ca77341ce88ef0eeaab37f2c0
出典データセット
uspto-grants-2012_05
特許番号
US08188117B2

関連ノート

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