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

HRID 1252086노트

반응식

HRID 1252086 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 3883065,8-Dihydroquinoline-5,8-dione수율 47.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-61b2da111cef40618307e90a8308941d
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04742059

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