Lithium hydroxide, monohydrate → 4-oxo-3H,4H,5H-pyrrolo[2,3-c]quinoline-1-carboxylic acid

HRID 1969993노트

반응식

HRID 1969993 반응식
O.[OH-].[Li+].[O:4]=[C:5]1[C:14]2[NH:15][CH:16]=[CH:17][C:13]=2[C:12]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[NH:6]1.C([C:20]([O-:22])=[O:21])C>C(O)C.O>[O:4]=[C:5]1[C:14]2[NH:15][CH:16]=[C:17]([C:20]([OH:22])=[O:21])[C:13]=2[C:12]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[NH:6]1

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 86627461HCID 86627461, 화합물

생성물 1

HCID 120650844-oxo-3H,4H,5H-pyrrolo[2,3-c]quinoline-1-carboxylic acid수율 101.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

1.64 g (39 mmol) of lithium hydroxide monohydrate is added to 1 g (3.9 mmol) of 4-oxo-4,5-dihydro-3H-pyrrolo[2,3-c]quinoline-1-ethyl carboxylate (synthesis 1) suspended in 45 mL of ethanol and 45 mL of water, and the solution is stirred for 17 h at 70° C. then 5 h at 100° C. The ethanol is evaporated under vacuum and distilled water is added. The aqueous solution is washed with ethyl acetate then acidified with acetic acid to pH 4-5. The precipitate that forms is filtered then dried under vacuum at 55° C. to give 0.9 g (100%) of 4-oxo-4,5-dihydro-3H-pyrrolo[2,3-c]quinoline-1-carboxylic acid in the form of a beige solid.

후처리

  1. custom5 h
  2. customat 100° C
  3. customThe ethanol is evaporated under vacuum
  4. distillationdistilled water
  5. additionis added
  6. washThe aqueous solution is washed with ethyl acetate
  7. filtrationThe precipitate that forms is filtered
  8. customthen dried under vacuum at 55° C.

출처 및 근거

ORD 기록
ord-30b33b656ab94966a4cf89f4cc120d46
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08426437B2

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