Monobasic potassium phosphate → 5,8-Dihydroquinoline-5,8-dione

HRID 2308947ノート

反応式

HRID 2308947 の反応式
[OH:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[N:7]2.P([O-])(O)(O)=[O:13].[K+].N(S([O-])(=O)=O)(S([O-])(=O)=O)[O].[K+].[K+]>CO.O>[N:7]1[C:8]2[C:9](=[O:13])[CH:10]=[CH:11][C:2](=[O:1])[C:3]=2[CH:4]=[CH:5][CH:6]=1

参加物

6

反応物 3

HCID 516951Monobasic potassium phosphateHCID 3032624Potassium nitrosodisulfonateHCID 135441757Quinolin-5-ol

生成物 1

HCID 3883065,8-Dihydroquinoline-5,8-dione収率 47.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 23.2 g of 5-hydroxyquinoline in 1600 ml of methanol in an ice bath was added a total of 36 g of potassium dihydrogen phosphate and 96 g of potassium nitroso disulfonate in 8.8 liters of water in five portions over a 1 hour period. The mixture was then stirred overnight at room temperature, followed by extraction with four 1500 ml portions of chloroform. The extracts were combined, dried, filtered through alumina and evaporated to dryness, giving 12.0 g of crude product. An analytical sample was prepared by crystallization from petroleum ether, mp 110° C.

後処理

  1. extractionfollowed by extraction with four 1500 ml portions of chloroform
  2. customdried
  3. filtrationfiltered through alumina
  4. customevaporated to dryness

出典と根拠

ORDレコード
ord-ad7559ae3c4144d18cc6537b4e9b745b
出典データセット
uspto-grants-1987_09
特許番号
US04692449

反応ノート

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