Methanol → 9-Chloro-3-methyl-5-piperidin-3-yl-5H-isoxazolo[4,3-c]quinolin-4-one hydroiodide

HRID 2212192

反応式

HRID 2212192 の反応式
[I:1][Si](C)(C)C.COC([N:10]1[CH2:15][CH2:14][CH2:13][CH:12]([N:16]2[C:25]3[CH:24]=[CH:23][CH:22]=[C:21]([Cl:26])[C:20]=3[C:19]3=[N:27][O:28][C:29]([CH3:30])=[C:18]3[C:17]2=[O:31])[CH2:11]1)=O.CO.C(OCC)C>ClCCl>[IH:1].[Cl:26][C:21]1[C:20]2[C:19]3[C:18](=[C:29]([CH3:30])[O:28][N:27]=3)[C:17](=[O:31])[N:16]([CH:12]3[CH2:13][CH2:14][CH2:15][NH:10][CH2:11]3)[C:25]=2[CH:24]=[CH:23][CH:22]=1

参加物

6

反応物 4

HCID 887MethanolHCID 3283Diethyl EtherHCID 85247Trimethylsilyl iodideHCID 99515613-(9-chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-piperidine-1-carboxylic acid methyl ester

生成物 1

HCID 219637129-Chloro-3-methyl-5-piperidin-3-yl-5H-isoxazolo[4,3-c]quinolin-4-one hydroiodide収率 97%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Add iodotrimethylsilane (1.87 mL, 13.16 mmol) to a solution of 3-(9-chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-piperidine-1-carboxylic acid methyl ester (2.06 g, 5.48 mmol) in dichloromethane (40 mL). Stir the solution at room temperature under nitrogen overnight. Add methanol (3.2 mL, 78.93 mmol) dropwise, and stir the reaction at room temperature for 30 minutes. Concentrate the reaction, add to diethyl ether, sonicate, and filtere. Dry the solids on a vacuum pump to give 2.36 g of the title compound as a tan solid, 97% yield. 1H NMR: consistent with structure. MS (ion spray) 318 (M+).

後処理

  1. customthe reaction at room temperature for 30 minutes
  2. concentrationConcentrate
  3. customthe reaction
  4. customsonicate
  5. customDry the solids on a vacuum pump

出典と根拠

ORDレコード
ord-769fcdf1cdd8433c89c93ffe0bcf8a88
出典データセット
uspto-grants-2006_09
特許番号
US07101891B2

関連ノート

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