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Lithium hydroxide, monohydrate → 6-(3-Methyl-5-pyridin-2-yl-3H-[1,2,3]triazol-4-ylmethoxy)-pyridazine-3-carboxylic acid

HRID 402405
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HRID 402405 반응식
O.[OH-].[Li+].C([O:6][C:7]([C:9]1[N:10]=[N:11][C:12]([O:15][CH2:16][C:17]2[N:18]([CH3:28])[N:19]=[N:20][C:21]=2[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=2)=[CH:13][CH:14]=1)=[O:8])C>O.C1COCC1.CO>[CH3:28][N:18]1[C:17]([CH2:16][O:15][C:12]2[N:11]=[N:10][C:9]([C:7]([OH:8])=[O:6])=[CH:14][CH:13]=2)=[C:21]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=2)[N:20]=[N:19]1
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참가 물질

6

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 573350986-(3-Methyl-5-pyridin-2-yl-3H-[1,2,3]triazol-4-ylmethoxy)-pyridazine-3-carboxylic acid ethyl ester

생성물 1

HCID 674986856-(3-Methyl-5-pyridin-2-yl-3H-[1,2,3]triazol-4-ylmethoxy)-pyridazine-3-carboxylic acid수율 67%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매
HCID 8028Tetrahydrofuran용매

실험 절차

A solution of lithium hydroxide monohydrate (130 mg, 3.06 mmol) in water (5 mL) was added dropwise to a suspension of 6-(3-methyl-5-pyridin-2-yl-3H-[1,2,3]triazol-4-ylmethoxy)-pyridazine-3-carboxylic acid ethyl ester (521 mg, 1.53 mmol) in THF (5 mL) and MeOH (0.5 mL). The reaction mixture was then stirred at room temperature for 2 h. The reaction mixture was then evaporated and the residue dissolved in water, acidified with HCl (1N), and the resulting precipitate filtered off to afford the title product (320 mg, 67%) as a white solid. MS: m/e=311.2 [M−H]−.

후처리

  1. customThe reaction mixture was then evaporated
  2. dissolutionthe residue dissolved in water
  3. filtrationthe resulting precipitate filtered off

출처 및 근거

ORD 기록
ord-b3832445e52349db86a92d97c6f1c61b
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08742097B2

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