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

HRID 1969993ノート

反応式

HRID 1969993 の反応式
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

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 86627461HCID 86627461、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-30b33b656ab94966a4cf89f4cc120d46
出典データセット
uspto-grants-2013_04
特許番号
US08426437B2

反応ノート

読み込み中…