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Sodium Hydroxide → 6-Amino-7-methyl-quinoline-5-carboxylic acid

HRID 245651
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반응식

HRID 245651 반응식
C[O:2][C:3]([C:5]1[C:6]2[CH:7]=[CH:8][CH:9]=[N:10][C:11]=2[CH:12]=[C:13]([CH3:16])[C:14]=1[NH2:15])=[O:4].[OH-].[Na+]>O1CCOCC1.CO>[NH2:15][C:14]1[C:13]([CH3:16])=[CH:12][C:11]2[N:10]=[CH:9][CH:8]=[CH:7][C:6]=2[C:5]=1[C:3]([OH:4])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 579901536-Amino-7-methyl-quinoline-5-carboxylic acid methyl ester

생성물 1

HCID 579901086-Amino-7-methyl-quinoline-5-carboxylic acid수율 54.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

To a solution of 550 mg (2.54 mmol) of 6-amino-7-methyl-quinoline-5-carboxylic acid methyl ester in 11 mL of dioxane and 0.5 mL of methanol, is added 6.4 mL (6.4 mmol) of an aqueous solution of NaOH 1N. The mixture is stirred at ambient temperature for 16 hours. The solvents are evaporated and water is added to the residue. The product is precipitated at pH 6 by addition of concentrated HCl, filtrated, washed with a minimum of water and dried on high vacuum pump. The yellow crude solid (282 mg) obtained is used directly in the next step; LC/MS: 203/204 (M+H)+.

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후처리

  1. customThe solvents are evaporated
  2. additionwater is added to the residue
  3. customThe product is precipitated at pH 6 by addition of concentrated HCl
  4. filtrationfiltrated
  5. washwashed with a minimum of water
  6. customdried on high vacuum pump

출처 및 근거

ORD 기록
ord-fda2c7b81488472fb562c1f93f27bcf4
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658801B2

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