Lithium hydroxide, monohydrate → 6-[3-(4-fluoro-phenyl)-5-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyridazine-3-carboxylic acid

HRID 402449노트

반응식

HRID 402449 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]([C:23]3[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=3)[N:19]=[N:20][C:21]=2[CH3:22])=[CH:13][CH:14]=1)=[O:8])C>O.C1COCC1>[F:29][C:26]1[CH:25]=[CH:24][C:23]([N:18]2[C:17]([CH2:16][O:15][C:12]3[N:11]=[N:10][C:9]([C:7]([OH:8])=[O:6])=[CH:14][CH:13]=3)=[C:21]([CH3:22])[N:20]=[N:19]2)=[CH:28][CH:27]=1

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 573356996-[3-(4-Fluoro-phenyl)-5-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyridazine-3-carboxylic acid ethyl ester

생성물 1

HCID 674982766-[3-(4-fluoro-phenyl)-5-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyridazine-3-carboxylic acid수율 99.4%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of lithium hydroxide monohydrate (163 mg, 3.88 mmol) in water (7 mL) was added dropwise to a suspension of 6-[3-(4-fluoro-phenyl)-5-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyridazine-3-carboxylic acid ethyl ester (694 mg, 1.94 mmol) in THF (7 mL). The reaction mixture was then stirred at room temperature for 30 min and was then evaporated and the residue dissolved in water, acidified with HCl (1N), and the resulting precipitate filtered off to afford the title product (635 mg, 99%) as a white solid. MS: m/e=328.3 [M−H]−.

후처리

  1. customwas then evaporated
  2. dissolutionthe residue dissolved in water
  3. filtrationthe resulting precipitate filtered off

출처 및 근거

ORD 기록
ord-73091c1fe7bc433f931cf90731fccb30
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08742097B2

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