Potassium Permanganate → HCID 12898485、化合物

HRID 1579393ノート

反応式

HRID 1579393 の反応式
[Mn]([O-])(=O)(=O)=[O:2].[K+].[N:7]1[CH:12]=[CH:11][CH:10]=[C:9]2[CH2:13][C:14]3[CH:20]=[C:19]([CH:21]([OH:25])[CH:22]([CH3:24])[CH3:23])[CH:18]=[CH:17][C:15]=3[O:16][C:8]=12>CC(C)=O>[C:21]([C:19]1[CH:18]=[CH:17][C:15]2[O:16][C:8]3=[N:7][CH:12]=[CH:11][CH:10]=[C:9]3[C:13](=[O:2])[C:14]=2[CH:20]=1)(=[O:25])[CH:22]([CH3:23])[CH3:24]

参加物

4

反応物 2

HCID 516875Potassium PermanganateHCID 21568412HCID 21568412、化合物

生成物 1

HCID 12898485HCID 12898485、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
20 °C

実験手順

11 g of potassium permanganate is added in small portions to a solution of 6 g of 1-(5H-[1]benzopyrano[2,3-b]pyridin-7-yl)-2-methyl-1 -propanol in 160 ml of acetone, and the mixture is stirred at 20°C for 3 hours. The reaction mixture is filtered, and the residue is washed thoroughly with chloroform. The filtrate and washings are concentrated, and the residue is purified by column chromatography on silica gel with chloroform as eluent, and further by recrystallization from acetone to give 7-isobutyryl-5-oxo-5H-[1]benzopyrano[2,3-b]pyridine melting at 155°-156°C.

後処理

  1. filtrationThe reaction mixture is filtered
  2. washthe residue is washed thoroughly with chloroform
  3. concentrationThe filtrate and washings are concentrated
  4. customthe residue is purified by column chromatography on silica gel with chloroform as eluent
  5. customfurther by recrystallization from acetone

出典と根拠

ORDレコード
ord-1f91f159dfe543b1ab0078d1a403e94a
出典データセット
uspto-grants-1976_01
特許番号
US03931199

反応ノート

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