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Sodium Hydroxide → 5-(Methoxymethyl)pyridine-2,3-dicarboxylic acid

HRID 1078085
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반응식

HRID 1078085 반응식
[CH3:1][O:2][CH2:3][C:4]1[CH:5]=[C:6]([C:14]([O:16]C)=[O:15])[C:7]([C:10]([O:12]C)=[O:11])=[N:8][CH:9]=1.[OH-].[Na+]>O>[CH3:1][O:2][CH2:3][C:4]1[CH:5]=[C:6]([C:14]([OH:16])=[O:15])[C:7]([C:10]([OH:12])=[O:11])=[N:8][CH:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 110966932,3-Pyridinedicarboxylic acid, 5-(methoxymethyl)-, dimethyl ester

생성물 1

HCID 109983115-(Methoxymethyl)pyridine-2,3-dicarboxylic acid수율 83.9%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
10 °C

실험 절차

A mixture of dimethyl 5-(methoxymethyl)-2,3-pyridinedicarboxylate (60.0 g, 0.25 mol) and 50% sodium hydroxide solution (50.0 g, 0.63 mol) in water is heated at 90°-110° C. for 2 hours under nitrogen while distilling off methanol and water. The reaction mixture is cooled to 10° C., treated with sulfuric acid to adjust the pH to 2.0 and filtered to obtain a solid. The solid is washed with water and vacuum dried to give the title product as a white solid (44.3 g, mp 161°-162° C.).

후처리

  1. temperatureis heated at 90°-110° C. for 2 hours under nitrogen
  2. distillationwhile distilling off methanol and water
  3. additiontreated with sulfuric acid
  4. filtrationfiltered
  5. customto obtain a solid
  6. washThe solid is washed with water and vacuum
  7. customdried

출처 및 근거

ORD 기록
ord-6f0ec720883847bc9a4ef99ee1a21e56
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05545835

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