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Lithium hydroxide, monohydrate → 4,5-Dimethyl-1-(quinolin-4-yl)-1H-pyrrole-3-carboxylic acid

HRID 1792812
ノート
印刷プレビュー

反応式

HRID 1792812 の反応式
O.[OH-].[Li+].C([O:6][C:7]([C:9]1[C:13]([CH3:14])=[C:12]([CH3:15])[N:11]([C:16]2[C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[N:19]=[CH:18][CH:17]=2)[CH:10]=1)=[O:8])C>O1CCCC1.O.Cl>[C:7]([C:9]1[C:13]([CH3:14])=[C:12]([CH3:15])[N:11]([C:16]2[C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[N:19]=[CH:18][CH:17]=2)[CH:10]=1)([OH:8])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 22024966Ethyl 4,5-dimethyl-1-(quinolin-4-yl)-1H-pyrrole-3-carboxylate

生成物 1

HCID 220249714,5-Dimethyl-1-(quinolin-4-yl)-1H-pyrrole-3-carboxylic acid

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 8028
Tetrahydrofuran
溶媒

実験手順

1.89 g (45 mmol) of lithium hydroxide monohydrate are added at a temperature in the region of 20° C. to 1.3 g (4.42 mmol) of 3-ethoxycarbonyl-4,5-dimethyl-1-(quinol-4-yl)-1H-pyrrole dissolved in 50 mL of tetrahydrofuran and 50 mL of water. After stirring at reflux for 42 hours, the reaction mixture is concentrated virtually to dryness under reduced pressure (2.7 kPa) to give a residue that is taken up in 41 mL of 1N hydrochloric acid. After filtering off and drying the solid residue at ambient pressure at a temperature in the region of 50° C., 1.1 g of 3-carboxy-4,5-dimethyl-1-(quinol-4-yl)-1H-pyrrole are obtained in the form of a whitish solid melting at approximately 238° C.

後処理

  1. temperatureat reflux for 42 hours
  2. concentrationthe reaction mixture is concentrated virtually to dryness under reduced pressure (2.7 kPa)
  3. customto give a residue that
  4. filtrationAfter filtering off
  5. dry with materialdrying the solid residue at ambient pressure at a temperature in the region of 50° C., 1.1 g of 3-carboxy-4,5-dimethyl-1-(quinol-4-yl)-1H-pyrrole

出典と根拠

ORDレコード
ord-2a5c448614724de781c0c90100dd80fc
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07078414B2

反応ノート

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