Lithium hydroxide, monohydrate → HCID 67189619, 화합물

HRID 551819노트

반응식

HRID 551819 반응식
[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

참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 67188173HCID 67188173, 화합물

생성물 1

HCID 67189619HCID 67189619, 화합물수율 95.2%

시약·촉매·용매 1

HCID 21892291Methanol tetrahydrofuran water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-60f476268b1444e8931e710c1c2513ad
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947834B2

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