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(5-Fluoro-6-methoxypyridin-3-yl)methanol → 5-Fluoro-6-methoxypyridine-3-carbaldehyde

HRID 385564
ノート
印刷プレビュー

反応式

HRID 385564 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:10][OH:11])[CH:5]=[N:6][C:7]=1[O:8][CH3:9]>ClCCl.[O-2].[O-2].[Mn+4]>[F:1][C:2]1[C:7]([O:8][CH3:9])=[N:6][CH:5]=[C:4]([CH:3]=1)[CH:10]=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 57815441(5-Fluoro-6-methoxypyridin-3-yl)methanol

生成物 1

HCID 447547845-Fluoro-6-methoxypyridine-3-carbaldehyde収率 90%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒3 回HCID 6344Dichloromethane溶媒3 回

実験手順

To a solution of 0.54 g of (5-fluoro-6-methoxypyridin-3-yl)methanol in 5 mL of dichloromethane, 1.5 g of manganese dioxide was added. The mixture was stirred at room temperature for 3 hours, thereto were then added 0.89 g of manganese dioxide and 4 mL of dichloromethane, and the mixture was stirred for 1 hour. Thereto were further added 1.5 g of manganese dioxide and 2 mL of dichloromethane, and the mixture was stirred at room temperature for 2 hours 30 minutes. After leaving overnight, the insoluble substance was filtered off, and the filtration residue was washed with chloroform. The solvent was distilled off under reduced pressure to obtain 0.48 g of 5-fluoro-6-methoxynicotinaldehyde as a yellow solid.

後処理

  1. stirringthe mixture was stirred for 1 hour
  2. stirringthe mixture was stirred at room temperature for 2 hours 30 minutes
  3. customAfter leaving overnight
  4. filtrationthe insoluble substance was filtered off
  5. washthe filtration residue was washed with chloroform
  6. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-56330486ba3a4994a1b974a44941248d
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367831B2

反応ノート

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