Methanol → HCID 86649400、化合物

HRID 80154

反応式

HRID 80154 の反応式
[CH3:1][O:2][NH2:3].C([O-])([O-])=O.[K+].[K+].[F:10][C:11]1[CH:18]=[C:17]([N:19]2[CH2:23][CH2:22][N:21]([C:24]3[CH:25]=[N:26][CH:27]=[CH:28][C:29]=3[CH3:30])[C:20]2=[O:31])[CH:16]=[CH:15][C:12]=1[CH:13]=O.CO>C(COC)OC.C(Cl)(Cl)Cl>[CH3:1][O:2][N:3]=[CH:13][C:12]1[CH:15]=[CH:16][C:17]([N:19]2[CH2:23][CH2:22][N:21]([C:24]3[CH:25]=[N:26][CH:27]=[CH:28][C:29]=3[CH3:30])[C:20]2=[O:31])=[CH:18][C:11]=1[F:10]

参加物

7

反応物 4

HCID 887MethanolHCID 4113O-MethylhydroxylamineHCID 11430Potassium CarbonateHCID 596361642-Fluoro-4-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzaldehyde

生成物 1

HCID 86649400HCID 86649400、化合物収率 9.1%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
40 °C

実験手順

O-Methyl-hydroxylamine (84 mg, 1.003 mmol) and K2CO3 (207 mg, 1.5 mmol) were added to a solution of 2-fluoro-4-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzaldehyde-(I-121a: 300 mg, 1.003 mmol) in dimethoxyethane (10 mL). The resulting mixture was heated to 40° C. for 2 hours. The reaction was monitored by TLC (5% MeOH in CHCl3). The reaction mixture was filtered, washed with CHCl3 and the filtrate was concentrated under reduced pressure to afford 30 mg of crude 2-Fluoro-4-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzaldehyde O-methyl-oxime, which was used in the next step without further purification.

後処理

  1. filtrationThe reaction mixture was filtered
  2. washwashed with CHCl3
  3. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-faec1e1876794e68b942d7f8dbe08414
出典データセット
uspto-grants-2014_09
特許番号
USRE045173E1

関連ノート

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