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Sodium Hydroxide → 6-Methyl-4-pyridazinecarboxylic acid hydrochloride

HRID 1880211
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HRID 1880211 반응식
Cl[C:2]1[N:3]=[N:4][C:5]([CH3:11])=[CH:6][C:7]=1[C:8]([OH:10])=[O:9].[OH-].[Na+]>CO.[Pd]>[CH3:11][C:5]1[N:4]=[N:3][CH:2]=[C:7]([C:8]([OH:10])=[O:9])[CH:6]=1
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참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 265992153-Chloro-6-methylpyridazine-4-carboxylic acid

생성물 1

HCID 553007686-Methyl-4-pyridazinecarboxylic acid hydrochloride수율 30.1%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a stirred solution of 3-chloro-6-methyl-pyridazine-4-carboxylic acid (500 mg, 2.89 mmol) in MeOH (50 mL) was added NaOH (395 mg, 9.85 mmol) in pellets, followed by 150 mg of Pd/C (10%). The reaction mixture was put under a H2 atmosphere for 3 hours (atmospheric pressure). The reaction mixture was filtered on celite, acidified with aq. HCl (pH=6), and concentrated under vacuo. Column chromatography (SiO2, CH2Cl2/MeOH 7/3) yielded 6-methyl-pyridazine-4-carboxylic acid (120 mg, 29%) as a brown solid.

후처리

  1. filtrationThe reaction mixture was filtered on celite
  2. concentrationconcentrated under vacuo

출처 및 근거

ORD 기록
ord-21d3e6e20703469f9e332bca55fef9ee
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318759B2

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