Lithium hydroxide, monohydrate → HCID 67189619、化合物

HRID 551819ノート

反応式

HRID 551819 の反応式
[NH:1]1[CH:5]=[C:4]([CH:6]2[CH2:10][CH2:9][N:8]([C:11]([N:13]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[N:16]([C:23]4[CH:32]=[CH:31][C:26]([C:27]([O:29]C)=[O:28])=[CH:25][CH:24]=4)[CH2:15][CH2:14]3)=[O:12])[CH2:7]2)[CH:3]=[N:2]1.O.[OH-].[Li+]>O1CCCC1.CO.O>[NH:1]1[CH:5]=[C:4]([CH:6]2[CH2:10][CH2:9][N:8]([C:11]([N:13]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[N:16]([C:23]4[CH:24]=[CH:25][C:26]([C:27]([OH:29])=[O:28])=[CH:31][CH:32]=4)[CH2:15][CH2:14]3)=[O:12])[CH2:7]2)[CH:3]=[N:2]1

参加物

4

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 67188173HCID 67188173、化合物

生成物 1

HCID 67189619HCID 67189619、化合物収率 95.2%

試薬・触媒・溶媒 1

HCID 21892291Methanol tetrahydrofuran water溶媒

実験手順

4.2 g of methyl 4-[4-{[3-(1H-pyrazol-4-yl)pyrrolidin-1-yl]carbonyl}-3,4-dihydroquinoxalin-1(2H)-yl]benzoate and 50 ml of a tetrahydrofuran/methanol/water 2/1/1 mixture are introduced into a 250 ml round-bottomed flask equipped with a magnetic stirrer and placed in an ice bath. 1.63 g of lithium hydroxide monohydrate are added and the reaction mixture is stirred at ambient temperature for 18 h. After evaporating the organic solvents, citric acid is added up to pH 5. The precipitate is filtered off and dried under vacuum. 3.87 g of 4-[4-{[3-(1H-pyrazol-4-yl)pyrrolidin-1-yl]carbonyl}-3,4-dihydroquinoxalin-1(2H)-yl]benzoic acid are obtained.

後処理

  1. customequipped with a magnetic stirrer
  2. customplaced in an ice bath
  3. customAfter evaporating the organic solvents, citric acid
  4. additionis added up to pH 5
  5. filtrationThe precipitate is filtered off
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-60f476268b1444e8931e710c1c2513ad
出典データセット
uspto-grants-2011_05
特許番号
US07947834B2

反応ノート

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