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Hydrochloric Acid → 6-Amino-5-iodo-2-(methyloxy)-3-pyridinecarboxylic acid

HRID 489805
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HRID 489805 반응식
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([C:10]([O:12]C)=[O:11])=[CH:4][C:3]=1[I:14].[OH-].[Li+].Cl>CO.O>[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([C:10]([OH:12])=[O:11])=[CH:4][C:3]=1[I:14]
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 22262635Methyl 6-amino-5-iodo-2-(methyloxy)-3-pyridinecarboxylate

생성물 1

HCID 222626676-Amino-5-iodo-2-(methyloxy)-3-pyridinecarboxylic acid수율 97.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매
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반응 조건

온도
70 °C

실험 절차

To a solution of methyl 6-amino-5-iodo-2-(methyloxy)-3-pyridinecarboxylate (1.4 g, 4.54 mmol) in methanol (30 ml), 1M aqueous lithium hydroxide (9 ml, 9 mmol) was added and the mixture was heated at 70° C. for 2 h. After cooling to room temperature, the mixture was concentrated in vacuo to give a solid. The residual solid was dissolved in water (50 ml) and acidified (pH=5) by addition of 2N aqueous hydrochloric acid. The resultant solid was collected by filtration, washed with water and dried in vacuo under 60° C. to give 1.3 g (92%) of the title compound.

후처리

  1. temperatureAfter cooling to room temperature
  2. concentrationthe mixture was concentrated in vacuo
  3. customto give a solid
  4. filtrationThe resultant solid was collected by filtration
  5. washwashed with water
  6. customdried in vacuo under 60° C.

출처 및 근거

ORD 기록
ord-356adbb358054d1b8c63afb83e93b00f
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06979690B2

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