Potassium Permanganate → HCID 13207925、化合物

HRID 1579381ノート

反応式

HRID 1579381 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>[O:2]=[C:13]1[C:9]2[C:8](=[N:7][CH:12]=[CH:11][CH:10]=2)[O:16][C:15]2[CH:17]=[CH:18][C:19]([CH:21]([OH:25])[CH:22]([CH3:23])[CH3:24])=[CH:20][C:14]1=2

参加物

4

反応物 2

HCID 516875Potassium PermanganateHCID 21568412HCID 21568412、化合物

生成物 1

HCID 13207925HCID 13207925、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

15 g of potassium permanganate is added in small portions to a solution of 11 g of 1(5H-[1]benzopyrano[2,3-b]pyridin-7-yl)-2-methyl-1-propanol in 200 ml of acetone, while the temperature is kept at 10°C. Then the mixture is allowed to stand at 20°C for 1 hour. The reaction mixture is filtered, and the crystalline residue is washed 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 ethanol to give 1-(5-oxo-5H-[1]-benzopyrano[2,3-b]-pyridin-7-yl)-2-methyl-1-propanol melting at 160°C.

後処理

  1. customis kept at 10°C
  2. filtrationThe reaction mixture is filtered
  3. washthe crystalline residue is washed with chloroform
  4. concentrationThe filtrate and washings are concentrated
  5. customthe residue is purified by column chromatography on silica gel with chloroform as eluent
  6. customfurther by recrystallization from ethanol

出典と根拠

ORDレコード
ord-910602d8487145259a524909548a6065
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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