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

HRID 1792805ノート

反応式

HRID 1792805 の反応式
O.[OH-].[Li+].C[O:5][C:6]([C:8]1[C:12]([CH3:13])=[CH:11][N:10]([C:14]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:17]=[CH:16][CH:15]=2)[CH:9]=1)=[O:7]>O1CCCC1.O>[C:6]([C:8]1[C:12]([CH3:13])=[CH:11][N:10]([C:14]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:17]=[CH:16][CH:15]=2)[CH:9]=1)([OH:7])=[O:5]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 22024954Methyl 4-methyl-1-(quinolin-4-yl)-1H-pyrrole-3-carboxylate

生成物 1

HCID 220249694-Methyl-1-(quinolin-4-yl)-1H-pyrrole-3-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

0.63 g (15 mmol) of lithium hydroxide monohydrate is added at a temperature in the region of 20° C. to 1.21 g (4.54 mmol) of 3-methoxycarbonyl-4-methyl-1-(quinol-4-yl)-1H-pyrrole dissolved in 50 mL of tetrahydrofuran and 50 mL of water. After stirring at reflux for 22 hours, the reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa) to give a residue which is taken up in 20 mL of water and then triturated with 15 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., 1.05 g of 3-carboxy-4-methyl-1-(quinol-4-yl)-1H-pyrrole are obtained in the form of a whitish solid. Mass spectrum (EI): EI: m/e 252 (M+.) m/e 207.

後処理

  1. temperatureat reflux for 22 hours
  2. concentrationthe reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa)
  3. customto give a residue which
  4. customtriturated with 15 mL of 1N hydrochloric acid
  5. filtrationAfter filtering off
  6. dry with materialdrying the solid residue at ambient pressure at a temperature in the region of 50° C., 1.05 g of 3-carboxy-4-methyl-1-(quinol-4-yl)-1H-pyrrole
  7. customare obtained in the form of a whitish solid

出典と根拠

ORDレコード
ord-f2bee4fff69a42e4b9e7a6127aaa4781
出典データセット
uspto-grants-2006_07
特許番号
US07078414B2

反応ノート

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